001484   VIJAYENDAR V, KRISHNA E V, MISRA S, JALA R C R (Academy of Scientific and Innovative Research, New Delhi - 110 001, Email: jrcreddy10@gmail.com) : Synthesis, cytotoxic evaluation of substituted cinnamic-based 1,2,4-triazolo thiadiazoles. Indian J Chem Sec B 2019, 58B(04), 475-81.

In an attempt to find a new class of cytotoxic agents, a series of 3,6-disubstituted-[1,2,4] triazolo[3,4-b] [1,3,4]thiadiazoles have been synthesized using undecenoic acid and various cinnamic acids. The structures of the synthesized compounds have been confirmed using ¹H and ¹³C NMR, IR and mass spectroscopy. The prepared compounds have been evaluated for their in vitro cytotoxic activities against four human cancer cell lines namely, HeLa, B16-F10, SKOV3, MCF7 and CHO-K1 Normal Cell line using MTT assay. Compounds 6a and 6h show promising activity against HeLa (IC₅₀ value 8.92 µM) and SKOV3 cell lines (IC₅₀ value 9.43 µM). Majority of the compounds show significant activities against HeLa cell line with the IC₅₀ values ranging from 8.92 to 13.44 μM. All the compounds show good activity against SKOV3 cell line with the IC₅₀ values ranging from 9.43 to 19.34 μM. Majority of the compounds are non toxic towards the Chinese hamster ovary (CHO-K1) normal cell line.

1 table, 46 ref

001476   SUHANA H, LABARAN M (Chemistry Dep, SRM Institute of Science and Technology, Kattankulathur - 603 203, Email: suhana.h@ktr.srmuniv.ac.in) : Synthesis of (3-chloro-1-phenylsulfonylindol-2-ylmethyl) methylamine. Indian J Chem Sec B 2019, 58B(03), 420-2.

Indoles are an important class of heterocyclic compounds with diverse biological activity. This is mainly because of the unique ability of the compounds to mimic the structure of peptides and bind reversibly to proteins. Therefore, efficient methodologies for the synthesis of various indole derivatives are always of interest to both organic and medicinal chemists. Although there have been several reports for the synthesis of 2-substituted indoles, most of the methods have several disadvantages such as expensive reagents, toxic solvents, harsh reaction conditions, tedious workup procedures and poor yield of products. In the present work, a simple and efficient method for the synthesis of a novel 2-substituted indole has been developed.

13 ref

001475   SUHANA H, IDRIS M A (Chemistry Dep, SRM Institute of Science and Technology, Kattankulathur - 603 203, Email: suhana.h@ktr.srmuniv.ac.in) : Synthesis of a novel 2-vinyl indole. Indian J Chem Sec B 2019, 58B(03), 416-9.

Selectively functionalized 2-vinyl indoles are synthetically active building blocks for the regio and stereo controlled construction of annelated indoles as well as carbazole alkaloids. Various pyrido carbazoles known to have significant antileukaemic activity have been synthesised photochemically from 2-vinyl indoles. A brief survey of literature revealed that there are several methods available for the synthesis of 2-vinyl indoles. In the present work, we herein report a simple and efficient route for the synthesis of a novel 2-vinyl indole. Earlier studies have shown that 1-phenylsulfonyl-2-methyl-3-phenylthioindole undergoes facile side chain bromination to afford 1-phenylsulfonyl-2-bromomethyl-3-phenyl thioindole. This compound is chosen as the starting material for the synthesis of the target molecule. The bromo compound is then converted to its phosphonate ester by heating with triethyl phosphite at 160°C. Then the phosphonate ester is converted to the desired compound namely 4-β-(N-phenylsulfonyl-3-phenylthioindol-2-yl) vinyl benzophenone via Wittig-Horner reaction with 4-benzoyl benzaldehyde. The bright yellow solid thus obtained is found to melt at 158-60°C. It is further characterized by infra-red, ¹H and ¹³C NMR, and mass spectral data. Detailed investigations on the biological activity of similar 2-vinyl indoles will be carried out.

16 ref

001401   DAS T C, QUADRI S A I, FAROOQUI M (Dr. Rafiq Zakaria Coll for Women, Aurangabad - 431 001, Email: mazahar_64@rediffmail.com) : Synthesis of new 4-substitued-1-(4-amino phenyl)-5,6-dihydropyridine-2(1H)-one sulfonamide conjugates and evaluation of their anti-microbial activity. Indian J Chem Sec B 2019, 58B(03), 371-80.

A new series of substituted sulfonyloxopyridine conjugates are reported for first time. The antibacterial and antifungal activities of the synthesized compounds have been evaluated against known bacterial strains. The obtained data indicated that in particular, compound 7a, i.e. N-(4-(3-(morpholin-2-oxo-5,6-dihydropyridin-1(2H)-yl]phenyl)benzenesulfonamide exhibited activity comparable to the well known antibacterial agents. The previously reported expensive and delicate processes for synthesis of 1-(4-nitrophenyl)piperidine-2-one 3 have also been replaced with novel and efficient processes via lactam ring activation.

1 illus, 3 tables, 19 ref

001472   SRIKRISHNA A, SATYANARAYANA G (Chemistry Dep, Indian Institute of Technology, Hyderabad, Kandi - 502 285, Email: gvsatya@iith.ac.in) : Facile enantiospecific syntheses of oxabicyclo[4.4.0]decene-diones from carvone via mild Lewis acid mediated lactonizations. Indian J Chem Sec B 2019, 58B(03), 362-70.

An efficient and concise enantiospecific syntheses of oxabicyclo[4.4.0]decene-diones have been accomplished starting from carvone. This strategy is a chiron based approach by making use of mild Lewis acid mediated intramolecular lactonization as key step for the formation of fused bicyclic lactones. Notably, these bicyclic lactones constitute bicyclic carbon framework of diterpene natural products.

11 ref

001471   SRIKRISHNA A, SATYANARAYANA G (Chemistry Dep, Indian Institute of Technology, Hyderabad, Kandi - 502 285, Email: gvsatya@iith.ac.in) : Enantiospecific syntheses of oxacyclodecanes from carvone via mild Lewis acid mediated etherifcation. Indian J Chem Sec B 2019, 58B(03), 353-61.

An efficient enantiospecific syntheses of oxatri-/tetra-cyclodecanes have been accomplished starting from (R)-carvone. A mild Lewis acid (BF₃^.OEt₂) mediated intramolecular etherification is used as the key step. Structurally aesthetic tri- and tetracyclic ethers have been synthesized.

13 ref

001478   SULEYMANOVA F, NESTEROVA O, MATYUSHIN A (Chemistry Dep, Sechenov First Moscow State Medical Univ, Moscow, Russia, Email: suleymanovafidan5@gmail.com) : HPLC quantification of hydroxycinnamic and organic acids of Canadian goldenrod (Solidago canadensis L.). Pharmacogn J 2019, 11(2), 400-4.

Canadian goldenrod (Solidago canadensis L.) is a medicinal plant widely used in traditional medicine across the world for several hundred years. According to literature data, S. canadensis contains various groups of biologically active substances, including tannins, flavonoids, etc. The aim of the study was to identify and quantify hydroxycinnamic and organic acids in aerial parts of Canadian goldenrod, as these groups of substances demonstrate a broad spectrum of therapeutic activities. Ethanolic extracts of S. canadensis, gathered in Central Russia, were analyzed using Highperformance liquid chromatography (HPLC). Hydroxycinnamic acids (HCA) determination was carried out by HPLC method with UV detection at 330 nm using HCA Reference standards (RS). Organic acids (OA) determination was performed in the same manner, utilizing UV detection at 210 nm and corresponding OA RS. It was established that S. canadensis HCA composition is represented by cichoric, caffeic, chlorogenic, quinic and ferulic acids. The total HCA content in was 1.16 g ± 10.7 mg / 100 g. Main OA, found in S. canadensis, are ascorbic, citric, tartaric, succinic, gallic, malic, oxalic and fumaric acids, with the total OA content of 426.5 mg ± 6.4 mg / 100 g. The described HPLC method was successfully used for analysis of S. canadensis aerial parts ethanolic extracts. The method can be utilized for HCA and OA identification and quantification in both herbal raw material and herbal medicinal products containing Canadian goldenrod.

2 illus, 2 tables, 27 ref

001480   SYAKFANAYA A M, SAPUTRI F C, MUN’IM A (Indonesia Univ, West Java, Indonesia, Email: munim@farmasi.ui.ac.id) : Simultaneously extraction of caffeine and chlorogenic acid from Coffea canephora bean using natural deep eutectic solvent-based ultrasonic assisted extraction. Pharmacogn J 2019, 11(2), 267-71.

NADES is an alternative solvent in the extraction of metabolites from plants which has many environmental benefits, such as low toxicity, biodegradability, can dissolve polar and non-polar compounds, low costs and simple preparation. This study aims to determine the effect of natural deep eutectic solvent-based ultrasonic-assisted extraction (NADES-UAE) on enrichment of caffeine and chlorogenic acid in extract from green coffee beans (Coffea canephora). The powders were extracted using NADES-UAE method in several types of extraction condition, including the composition of NADES, water addition in NADES and extraction time. Caffeine and chlorogenic acid content were analyzed using HPLC, reverse phase system and C₁₈ ODS-3 column. The highest of caffeine and chlorogenic acid content was respectively, 7.89 mg/g and 28.62 mg/g (composition of NADES betaine: sorbitol [1:1.2] ratio and NADES-water addition [1:2] ratio for 30 min). This research showed that the composition of NADES, extraction time and water addition are important parameter in extracting caffeine and chlorogenic acid content in green coffee beans.

4 illus, 3 tables, 18 ref

001419   HUDA P, BISHNOI A, FATMA S, DEVI P, VERMA A K (Chemistry Dep, Lucknow Univ, Lucknow - 226 007) : Synthesis and spectral analysis of 4-(4-chlorophenyl)-3,4,6,7,8,9-hexahydro-1H-cyclohepta-pyrimidin-2(5H)-one and study of its quantum chemical and thermodynamic properties. Indian J Pure Appl Phys 2019, 57(4), 250-60.

In this article the synthesis and spectral analysis of a novel compound 4 (4-(4-chlorophenyl)-3,4,6,7,8,9-hexahydro-1H-cyclohepta-pyrimidin-2(5H)-one) has been deliberated. The aim of the synthesis is to obtain biologically active pyrimidin-2-one scaffold and to correlate its quantum chemical properties with its experimental results. The structure of the compound has been characterized by using different spectral analysis. The chemical calculations have been computed with the help of DFT level of theory using Becke3–Lee–Yang–Parr (B3LYP))/6-31G(d,p) basis set. DFT computed total first static hyperpolarizability β_tot =3.1686 ×10^-30 esu, indicates that the molecule could be an area of interest as an attractive future NLO material. Electrophilic and nucleophilic regions have been identified with the help of MESP plot. For the analysis of thermal behaviour of compound 4, thermodynamic properties such as heat capacity, entropy and enthalpy change at various temperatures have been calculated. A close examination of various structural and thermodynamic parameters such as electrostatic potential, electrophilicity (ω), chemical potential (µ), chemical hardness (η) and maximum amount of electronic charge transfer (∆Nmax) have been done for the compound 4. The local reactivity descriptors show that C(9) is the most reactive site for nucleophilic attack. In addition to it a discussion about correlation graphs between experimental and calculated ¹HNMR and ¹³CNMR spectroscopic values have also been done.

9 illus, 10 tables, 48 ref

001430   KUMAR A, RANI R, SHARMA T, BAMEZAI R K (Chemistry Dep, Jammu Univ, Jammu - 180 006) : Effect of concentration and temperature variations on interactions in (L-serine/L-valine + aqueous glucose/sucrose/lactose) systems: Viscometric and activation parametric study. Indian J Pure Appl Phys 2019, 57(4), 225-35.

Viscosities of (L-serine/L-valine + 0.1 mol dm^-3 aqueous glucose/sucrose/lactose) systems have been measured as a function of molal concentration of amino acids at different temperatures; 293.15 K, 298.15 K, 303.15 K, 308.15 K and 313.15 K. The viscosity data has been utilized to determine viscosity B-coefficients employing Jones-Dole equation. The viscosity B-coefficients of transfer (Δ_trB), variation of B with temperature (dB/dT) and solvation number (S_n) of L-serine/L-valine have been obtained using the experimental viscosity values. Further, Gibbs free energy of activation of viscous flow per mole of solvent (Δµ^°) as well as per mole of solute (Δµ^°) along with activation enthalpy (ΔH^°) and entropy (ΔS^°) have been computed using Feakin’s transition state theory to throw light on the mechanism of viscous flow. The results have been discussed in terms of solute-solvent interactions; and structure making tendency of amino acid molecules in aqueous saccharides solutions.

5 illus, 4 tables, 47 ref

001428   KARIPER I A (Erciyes Univ, Kayseri, Turkey) : Crystalline TeO₂ thin film with chemical bath deposition. Indian J Pure Appl Phys 2019, 57(3), 175-9.

Tellurium oxide (TeO₂) crystalline thin film has been produced with chemical bath deposition on substrates (commercial glass). Some properties of the films have been investigated by UV/VIS. The spectrum has been studied in terms of as transmittance, refractive index and reflectivity. The monoclinic and orthorhombic forms have been observed for the structural properties in XRD. The structural and optical properties of tellurium oxide thin films have been analyzed at different pHs of the chemical bath. EDX analysis has been used to determine the elemental ratio of tellurium in the films. Some properties of the films change with deposition pH. The concentration of sodium hydroxide was scanned at 2.5×10^-3 M, 5×10^-3 M, 7.5×10^-3 M and 10×10^-3 M at pHs of 10, 11, 11.50 and 12, respectively. The optical properties of the films change with the deposition pH of the chemical bath. Also, the film thickness changes with deposition pH at 12, 11.50, 11 and 10 and the respective thickness values are 900, 586, 657 and 866 nm. The optimum parameters have been determined with 10 mL 2.5×10^-3 M tellurium tetrachloride, 10 mL 2.5×10^-3 M of potassium hydroxide and 2 mL hydrogen peroxide at pH: 10 for producing γ-TeO₂.

8 illus, 1 table, 13 ref

001405   DEZENA R M B, MAURI R, BARROS F A P, ROSA P C P (Pharmacology Dep, State Univ Campinas, Campina, Brazil, Email: renan_marcel@hotmail.com) : Characterization of indole-3-acetic acid in cambial zone tissue by ultra-performance liquid chromatography-tandem mass spectrometry. J Appl Biol Biotechnol 2019, 7(2), 64-70.

The developmental plasticity of plants according to changes in their growth conditions is mediated by signaling molecules called hormones. The major classes of plant hormones are auxin, gibberellins, abscisic acid, and ethylene. Among these, the most important is indole-3-acetic acid (IAA). Quantification of IAA in an extract of approximately 10 mg obtained from the cambial zone of Eucalyptus leaves was performed by ultra-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC/ESI-MS/MS). The leaves were extracted using acetone, and the extract was analyzed using a reverse-phase column (Acquity UPLC BEH C18, 2.1 mm × 100 mm, 1.7 µm) at a flow rate of 0.2 mL/min with gradient elution of an aqueous mobile phase (containing 0.1 % formic acid) with methanol. This gradient elution provided an excellent performance in terms of specificity/selectivity, linearity, precision, and ruggedness/stability. In addition, the run time was short (6 min), with excellent linearity (R² > 0.99) in the range of 10–70 ng/mL. The structure of IAA was elucidated using UPLC/ESIMS/MS, operating and quantifying in multiple reaction monitoring (MRM) mode.

7 illus, 7 tables, 21 ref

001440   MOCHAMAD L, HERMANTO B, HESTIANAH E P (Airlangga Univ, Surabaya 60115, Indonesia, Email: lazuardi@fkh.unair.ac.id) : Determination of progesterone compounds in the crude methanol extract of Benalu duku leaves. Vet World 2019, 12(3), 358-66.

Dendrophthoe pentandra L. Miq (benalu duku) is a parasitic herb that commonly grows on the host plant Lansium domesticum. Researchers have found that the plant contains anticancer compounds and may contain phytoandrogens, including progesterone-like compounds, in its crude methanol extract. The objective of the current study was to investigate the compound of phyto progesterone in benalu duku leaves after extracted by methanol and prepared using an analytical column of high-performance liquid chromatography (HPLC). About 400 g of benalu duku leaves were pulverized, and their compounds were isolated by the isocratic method using an RP-18 analytical column (5 µm) with a mobile phase of 70:30 (methanol: water) in a photodiode array detector adjusted to 254 nm. The phyto progesterone compound was identified at a retention time of approximately 6.01 min. By LC-electrospray ionization mass spectrometry focusing on molecular fractions, the fingerprint area of the Fourier transform-infrared spectroscopy (FT-IR, cm⁻¹) and Hnuclear magnetic resonance (NMR) spectra indicated that the phyto progesterone product isolated was identical to the certified reference material of pure progesterone, particularly the specific functional groups in the FT-IR spectrum at wavenumbers of 1317.43 cm⁻¹ and 1386.86 cm⁻¹ and in the proton HNMR spectrum at carbon 21 of progesterone (p<0.05). Each 49.888 µg/mL of crude benalu duku leaf extract dissolved in the mobile phase contained 28.515 ± 0.713 µg/mL phyto progesterone.

8 illus, 2 tables, 36 ref

001473   SRINIVASAN S, PRIYA V (Botany Dep, PSG Coll of Arts & Science, Coimbatore, Tamil Nadu) : Phytochemical screening and GC-MS analysis of Cyperus dubius, Rottb. (Cyperaceae). J Med Plants Stud 2019, 7(2), 89-98.

In the present study the investigation on phytochemical screening was carried along with GC-MS analysis to identify the phyto-constituents present in extracts of Cyperus dubius, Rottb. Phytochemical analysis in different extracts (methanol, hexane) revealed the presence of secondary metabolites like alkaloids, flavonoids, phenols, terpenoids, glycosides, Phytoserols, quinone. Whereas, the GC-MS analysis showed 30 peaks indicates the presence of 30 compounds and among these Stigmast-5-en-3-ol, (3.beta.)-[31.39 %] was found to be major compound followed by Stigmasterol (9.40 %), Guanosine (6.44 %), Ergost-5-en-3-ol, (3.beta.)-(6.39 %), Olivetol, dimethyl ether (5.75 %), 1,3,4,5-tetrahydroxycyclohexanecarboxylic acid (4.39 %), 2-methyl-2-[2-(2,6,6-trimethyl-3-methylene-cyclohex-1-enyl)- vinyl]-[1,3]dioxolane (4.14 %), 9-octadecenoic acid (Z)-(3.96 %), Methyl commate C (3.91 %), 2,5- dimethoxybenzylamine (3.73 %), 4-formyl-2-methoxyphenyl acetate (3.47 %) and Gamma.-tocopherol (2.99 %) which possess pharmacologically and industrially potential phyto compounds like antioxidants, phytosteroids and number of unsaturated fatty acids.

1 illus, 4 tables, 33 ref

001466   SIWE G T, ERNESTINE N Z, MAHARJAN R, AMANG A P, MEZUI C, CHOUDHARY M I, TAN P V (Animal Biology & Physiology Dep, Yaoundé I Univ, Yaoundé, Cameroon) : Comparative GC-MS analysis of two crude extracts from Eremomastax speciosa (Acanthaceae) leaves. J Med Plants Stud 2019, 7(2), 25-9.

This study was designed to identify the possible volatile compounds present in two extracts from Eremomastax speciosa leaves. The air-dried leaves were powdered and subjected to extraction using respective solvents; distilled water and methanol/methylene chloride. Then, each of the extracts was further subjected to gas chromatography–mass spectrometry (GC-MS). GC-MS analysis revealed the presence of 22 compounds in aqueous extract and 44 compounds in methanol/methylene chloride extract. Five compounds were found commonly in both extracts. The major constituents identified in aqueous extract were olean-12-en-3-one (28.37 %), 2, 7-Dioxaisotwistane (19.77 %), 9-oxabicyclo [3.3.1] nonane2, 6-diol (15.80 %) and α-Amyrin (12.09 %). In methanol/methylene chloride extract the major compounds identified were n-hexadecenoic acid (17.74 %), stigmasterol (12.81 %), γ-sitosterol (10.50 %) and α-Linolenic acid (9.01 %). Some of these compounds were already reported to be pharmacologically active. From these results and given that Eremomastax speciosa is widely used to threat or prevent many diseases, it is obvious that this plant contains many biologically active compounds and might be exploited for the development of plant-based drugs.

2 illus, 2 tables, 19 ref

001426   KANTH M L, KAMAL B R (Mewar Univ, Chhitorgarh - 312 901, Email: kanthmsc06@gmail.com) : Development and validation of RP-HPLC for estimation of Neratinib in bulk and tablet dosage form. Int J Pharm Sci Drug Res 2019, 11(2), 56-60.

An accurate RP-HPLC method developed for the estimation of Neratinib in bulk and tablet dosage form. The method is and validatedfor parameters linearity, accuracy, suitability, specificity, precession, LOD, LOQ and robustness. An Altima column (150 mm ×4.6 mm ×5 μ) used for chromatographic separation within a runtime of 6 min. The mobile phase buffer (monopotassium phosphate) and acetonitrile (60:40 v/v) with 0.1 % formic acid is used. The flow rate maintained at 1.0 ml/min with the effluentsmonitored at 215 nm. The Neratinib analyzed at retention time of 4.001. The concentration linear over 30-180 μg/ml with regression equation y = 6065.6x + 795.43 and regression co-efficient 0.999.

7 illus, 7 tables, 14 ref

001454   PRABHA T, GRACE A C, SASIKALA S, MURUGESAN J (Pharmaceutical Analysis Dep, Nandha Coll of Pharmacy, Erode - 638 052, Email: drtpappa@yahoo.com) : Development and validation of RP-HPLC method for the estimation of doxofylline and terbutaline in pure and in its formulation. Int J Pharm Sci Res 2019, 10(4), 1981-7.

A new simple, rapid, and sensitive reversed-phase liquid chromatographic method was developed for the estimation of doxofylline and terbutaline in the tablet dosage form. The chromatographic separation was achieved on ODS C₁₈column (150 × 4.6 mm, 5 µm) at ambient temperature and effluent monitored at 257 nm. The mobile phase consists of ammonium acetate buffer (pH adjusted to 3 with o-phosphoric acid) and acetonitrile in the ratio of 50:50 v/v. The flow rate was maintained at 1 ml/min. The method was validated concerning linearity, precision, accuracy, ruggedness, limit of detection, limit of quantification and robustness. The assay methods were found to be linear from 16-96 µg/ml for doxofylline and 0.2-1.2 µg/ml for terbutaline. All validation parameters were within the acceptable range. The mean recovery was 99.35 and 99.25 for doxofylline and terbutaline respectively. The % RSD value was found to be less than 2. The limit of detection and limit of quantification for doxofylline and terbutaline were found to be 0.06 μg/ml and 0.024 μg/ml and 0.21 μg/ml and 0.079 μg/ml respectively. The result of the study showed that the proposed RP-HPLC method for the simultaneous estimation of doxofylline and terbutaline in the tablet dosage form is simple, accurate, sensitive, precise, specific and rapid which is useful for routine analysis of doxofylline and terbutaline in its formulations.

5 illus, 6 tables, 33 ref

001477   SUJANA K, SATYANARAYANA V (Pharmaceutical Analysis Dep, Acharya Nagarjuna Univ, Guntur - 522 510, Email: sujana_36@yahoo.co.in) : Validated stability indicating RP-HPLC method for simultaneous estimation of daunorubicin and cytarabine in bulk and its pharmaceutical dosage form. Int J Pharm Sci Res 2019, 10(4), 1895-901.

This paper describes a new validated Reverse-Phase HighPerformance Liquid Chromatography (HPLC) method for the simultaneous determination of two anti-cancer drugs, Daunorubicin and Cytarabine (Ara-C). A simultaneous determination method saves cost and time as both drugs can be injected into a single HPLC system without the need to change or re-equilibrate with a new mobile phase. The objective of the study is to develop a simultaneous determination method of two anti-cancer drugs, Daunorubicin and Cytarabine. The mobile phase consists of a mixture (55:45 v/v) of 0.1% OPA: acetonitrile at a flow rate of 0.8 ml/min, with a PDA detector at 240 nm. Separation was achieved on a kromosil C-18 column (5 µm; 250 mm × 4.6 mm) maintained at 30 °C temperature in a column oven. The method was linear between 7.25 µg/mL - 43.5 µg/mL for Daunorubicin and 16.2 µg/Ml - 97.5 µg/mL for Cytarabine. The limit of detection was 0.29 µg/mL for Daunorubicin, and 1.15 µg/mL for Cytarabine and the limit of quantification was 0.88 µg/mL for Daunorubicin and 3.47 µg/mL for Cytarabine. The developed RP-HPLC method achieved good precision and accuracy. The developed and validated method was suitable to be used for routine analysis of Daunorubicin and Cytarabine.

10 illus, 10 tables, 11 ref

001459   SANKAR P R, SWATHI V, BABU P S (Pharmaceutical Analysis and Quality Assurance Dep, Vignan Pharmacy Coll, Vadlamudi - 522 213, Email: banuman35@gmail.com) : Development and validation of novel UV and RP-HPLC methods for determination of cilnidipine (a new generation Ca channel blocker) in pharmaceutical dosage form. Int J Pharm Sci Res 2019, 10(4), 1886-94.

An accurate and precise High-Performance Reversed-Phase Liquid Chromatographic and UV spectrophotometric methods were developed and validated for the quantitative determination of Cilnidipine, a novel generation Ca channel blocker in the pharmaceutical dosage form. Good quality chromatographic separation of Cilnidipine was carried out by using thermo scientific model C18 Column (4.6 mm i.d. × 250 mm, 5 µm particle size) (based on 99.999 % ultra-high purity silica) using mobile phase consisting acetonitrile: methanol (50:50 % v/v) at flow rate of 1.0 mL/min. The λ_max of the Cilnidipine in methanol (as a solvent) was found to be 242 nm. The drug following linearity in the concentration range of 2-10 µg/mL with a correlation coefficient value of 0.9999 for both UV and HPLC methods. The regression equation for Cilnidipine UV method was found to be Y = 0.081x + 0.0017 and for HPLC method was Y = 25517x - 4755. LOD and LOQ were found as 0.15095 µg/mL and 0.45742 µg/mL for UV method and for HPLC method it was found to be 0.003 µg/mL and 0.0099 µg/mL. The developed methods were validated in pursuance of ICH Q2 (R1) guidelines. Both the methods were linear, precise, accurate with recoveries in the range of 98-102 % and low values of % RSD are indicative of the accuracy of the method. The detailed quantitative results of this study show that this method is simple, quick, precise, accurate, sensitive, cost-effective and robust. Thus, the developed UV and gradient RP-HPLC method can be successfully applied for the routine quality control analysis in pharmaceutical dosage forms.

12 illus, 4 tables, 15 ref

001399   DAMLE M, CHOUDHARI S (Quality Assurance Dep, All India Shri Shivaji Memorial Society’s Coll of Pharmacy, Pune - 411 001, Email: mcdamle@rediffmail.com) : Development and validation of stability indicating HPLC method for estimation of salmeterol xinafoate. Int J Pharm Sci Res 2019, 10(4), 1865-9.

Simple, rapid validated stability-indicating HPLC method for estimation of Salmeterol xinafoate was successfully developed. The separation was achieved by using a mobile phase of buffer: methanol in the ratio of 60:40 v/v using HiQ SiL C18 column (150 × 4.6 mm i.d. 5 μm) at 1.2 mL/min as flow rate. The detection was carried out at 252 nm using a PDA detector. The retention time observed was 11.89 ± 0.3 min. This drug was subjected to stress conditions as per ICH Q1A (R2). Linearity was found to be in the concentration range of 10-50 μg/mL with r² = 0.9958. The suitability of this HPLC method for quantitative estimation of Salmeterol xinafoate was proved by validation by the requirements of ICH guidelines Q2A (R1).

5 illus, 6 tables, 10 ref

001439   MISAL N V, CHEMATE S Z (Pharmaceutics Dep, Dr. V.V.P.F’s Coll of Pharmacy, Ahmednagar - 414 111, Email: nileshmisal171@gmail.com) : Formulation and evaluation of lornoxicam mouth dissolving tablet by using natural superdisintegrants. Int J Pharm Sci Res 2019, 10(4), 1848-55.

The concept of fast dissolving drug delivery system emerged from the desire to provide patients with more convenient means of taking their medication. It is difficult for many patients to swallow tablets and hard gelatin capsules. The main objective of the study is to develop a reproducible formulation of fast dissolving tablets of Lornoxicam already used the therapeutic molecule to enhance effectiveness and to avoid side effects (gastric irritation) of the drug. Different batches of tablets were prepared by direct compression method using a different concentration of superdisintegrants like gum karaya, chitosan, and fenugreek seed mucilage powder. Before compression pre-formulation studies were done which includes characterization of the blend and physical compatibility studies with excipients. Effect of change in super disintegrant and their concentration on the formulation was studied. Final batches were compared for the superiority of superdisintegrants in the formulation of MDT of Lornoxicam. Tablets were evaluated for weight variation, thickness, hardness, friability, drug content, in-vitro disintegrating time and in-vitro drug release.

9 illus, 7 tables, 10 ref

001437   MARUTHI R, CHANDAN R S, RAIKAR P (Pharmaceutical Chemistry Dep, JSS Coll of Pharmacy, Mysuru - 570 015, Email: maruthireddy666@gmail.com) : Simultaneous estimation and analytical method development, validation for the teneligliptin and metformin by RP-UFLC. Int J Pharm Sci Res 2019, 10(4), 1811-9.

The study aims to develop an analytical method for the simultaneous estimation of Teneligliptin and Metformin using RP-UFLC. A simple, sensitive and accurate method was developed for Teneligliptin and Metformin using the chromatographic conditions of C18 Phenomenex Kinetex (250 mm × 4.6 mm i.e., 5 μm particle size) column in gradient elution mode with the mobile phase consisting of methanol, acetonitrile and potassium dihydrogen orthophosphate adjusted to pH 4.6 using orthophosphoric acid (40:20:40) with a flow rate of 1.0 mL/min, injection volume 10 µl and the eluent was detected at 250 nm using PDA and UV detector. The retention time of Teneligliptin and Metformin were found to be 5.2 min and 2.5 min respectively. The above method was validated concerning system suitability, linearity, precision, limit of detection (LOD) and limit of quantification (LOQ), accuracy (recovery) and robustness according to ICH guidelines. The linearity of the above methods was found to be 2-10 µg/mL for Teneligliptin and 25-125 µg/mL for Metformin. Hence, these methods can be used for routine analysis in quality control laboratories.

7 illus, 12 tables, 26 ref

001449   PANDEY A K, DWIVEDI D (Chemistry Dep, Pt. S.N.S. Govt P.G. (Auto) Coll, Shahdol - 484 001, Email: akpandeybspr@gmail.com) : Oxidative determination of some antihistamine drugs in pure form and their pharmaceutical preparations by using pyridinium fluoro chromate (PFC) reagent. Int J Pharm Sci Res 2019, 10(4), 1787-94.

In this paper Chromium (VI) based Pyridinium fluoro chromate (PFC) reagent has been used as an oxidant for the determination of some antihistamine drugs e.g. Promethazine hydrochloride (PMH) and Pheniramine maleate (PM) in pure form and their pharmaceutical preparations such as Phenergan (Injection and tablet) and Avil (Tablet and injection) respectively. The main principle of this method is based on the fact, that each pharmaceutical drug contains a specific organic functional group, which on oxidation in the presence of selected oxidant (Here PFC is used as an oxidant) provides the new oxidized product. This type of oxidation reaction between the drug molecule and an oxidant establishes a stoichiometric relationship between the drug molecule and an oxidant. This relationship is the basis of quantitative estimation of drugs in pure form and their pharmaceutical preparations. In this research, oxidizing reagent Pyridinium fluoro chromate (PFC) oxidizes the sulfur atom of Promethazine hydrochloride (PMH) to the corresponding sulphoxide, whereas in case of Pheniramine maleate (PM) it oxides one hydroxyl (-OH) group of carboxylic (-COOH) group to corresponding aldehydic (-CHO) group. Thus an oxidant PFC establishes a 1:1 ratio with both Promethazine hydrochloride (PMH) and Pheniramine maleate (PM) drug. Oxidative determination of these drugs was carried out by adopting the iodometric titration (Visual volumetric) method. The applied technique was very simple, convenient, accurate, precise and economical. To examine the accuracy and precision of results various statistical analysis such as percentage error, standard deviation (SD) and coefficient of variation (CV) was also calculated for each sample. The proposed method was validated by recovery analysis, by drug addition method.

4 illus, 3 tables, 28 ref

001482   TOPLE J S, SHERJE A, MALLYA R (Quality Assurance Dep, Dr. Bhanuben Nanavati Coll of Pharmacy, Mumbai - 400 052, Email: jeevankala.tople@gmail.com) : Analytical method development and validation for simultaneous determination of pyrantel pamoate and febantel in an oral dosage form by high-performance liquid chromatography (HPLC). Int J Pharm Sci Res 2019, 10(4), 1747-52.

The present manuscript describes a new simple, specific, precise and accurate RP-HPLC development and subsequent validation for simultaneous estimation of Pyrantel pamoate and Febantel in their combined dosage form. The proposed method involves the utilization of a hypersil BDS C18 (150 × 4.6 mm, 5 µ) column, mobile phase containing acetonitrile: phosphate buffer in the ratio 85:15% v/v and 55:45% v/v with apparent pH adjusted and maintained to 3.5 using 0.01M orthophosphoric acid, pumped at a flow rate of 1.0 ml/min. The injection volume was 20 µl, and detection was monitored at 286 nm. The components were eluted by gradient mode. The peaks obtained were sharp and well resolved with retention times 4.5 min (Pyrantel pamoate) and 6.5 min (Febantel). The calibration curves were linear (r² =0.999) over the concentration range of 25-150 µg/mL for Pyrantel pamoate and Febantel both. Validations of the proposed method were carried out for its accuracy, precision, linearity, robustness LOD and LOQ according to ICH Q2 R1 guidelines. The statistical analysis was carried out and the results of which were found satisfactory. Based on results, the developed method could be used for routine estimation Pyrantel pamoate and Febantel in the marketed formulation.

6 illus, 8 tables, 12 ref

001389   ANBAZHAKAN K, PRAVEENA R, SADASIVAM K (Chemistry Dep, Bannari Amman Institute of Technology, Sathyamangalam - 638 401, Email: praveethang@gmail.com) : Methylation effect of apigenin 8-C-glucoside towards antioxidant potential - A DFT study. Int J Pharm Sci Res 2019, 10(4), 1734-40.

The extensive study on O - methylated flavonoids reveals that substitution with methyl group enhances the radical scavenging behavior in certain compounds. Due to potential applications of C-glycosides in metabolic engineering, methylation in these flavonoids needs to be analyzed in both theoretical and experimental levels for their radical scavenging behavior. In this work naturally occurring C- glycosyl flavonoid apigenin 8-C-glucoside (vitexin) is theoretically simulated by substituting the C4′, C5 and C7 hydroxyl positions with methoxy unit and studied with the aid of density functional theory (DFT) for radical scavenging behavior. Structural stability is attained through B3LYP/6-311G(d,p) theory using Gaussian 03 package which provided the stable conformer for the studied compound without imaginary frequency. Structural activity is analyzed with the support of parameters like kinetic energy (temperature independent), HOMO-LUMO, molecular descriptors, Mulliken charge density analysis and compared with vitexin. Combined investigation of the parameters above revealed the superiority of phenyl hydroxyl vitexin over phenyl methoxy vitexin for radical scavenging activity unlike its O methylated flavonoids.

3 illus, 3 tables, 12 ref

001427   KANTHALE S B, THONTE S S, SUPEKAR B B (Swami Ramanand Teerth Marathwada Univ, Nanded - 431 606, Email: sangamkanthale@gmail.com) : Development of stability indicating assay method: A review. Int J Pharm Sci Res 2019, 10(4), 1625-31.

Stability of pharmaceuticals is defined as the ability to retain the quality, purity, Identity, and safety throughout the shelf life of products. It is of main concern because drug substance and products lose its Potency and quality after the time passes, due to change in environmental conditions such as temperature, light, and humidity. It is essential that quality of drugs should maintain throw out the life cycle of drug products for their safe and effective use. The need for constant monitoring of the drug substance and product for their quality and purity has the origin of the development of various stability testing methods. Stability testing now becomes a regulatory requirement for filing NDA and ANDA to USFDA and various regulatory agencies. Stability indicating methods had originated from advancement in various analytical instrument technologies. Stability indicating methods of drug substance and products have the ability for separation, identification, qualification, and quantification of all impurities associated with drug substance and drug product at any storage Conditions to give the exact concentration of drug substance or analyte at any time point over the shelf life of products and beyond. These are helpful to understand the degradation pathways as well as obtaining knowledge about impurities developed during processing which should not be present in drug products or have a specific limit, if present. The present review explored the importance, regulatory requirement, various analytical techniques used and some successfully developed stability indicating methods for different drug substance and drug products.

3 tables, 70 ref

001474   SRIVASTAVA A, MISHRA A P, CHANDRA S, BAJPAI A (Pranveer Singh Institute of Technology, Kanpur - 209 305, Email: srivastava457@gmail.com) : Benzothiazole derivative: A review on its pharmacological importance towards synthesis of lead. Int J Pharm Sci Res 2019, 10(4), 1553-66.

Heterocyclic chemistry plays a very most important role in medicinal chemistry as well as in organic chemistry. Most of the drug molecule formed and possesses therapeutic activity due to the heterocyclic scaffold. A slight change in heterocyclic moiety leads to the major therapeutic change in the drug molecule. Benzothiazole can serve as a unique and versatile moiety for experimental drug design. Benzothiazole and its derivatives are the essential chemical compounds with tremendous application in research area especially in synthetic as well as in pharmaceutical chemistry because of its potent and significant pharmacological activities. As we know that benzothiazole is a combination of two rings six-membered and five-membered and it is also known that both rings are responsible for the therapeutic activity. The main objective of our study is to find what changes lead to a better corrective benzothiazole shift moiety. A well-known approach to design new drug-like molecules, which allows achieving new pharmacological profile, action, toxicity lowering, is the development of a combination of 2- aminobenzothiazoles with another heterocyclic ring. A literature search was conducted on the databases namely Science direct, and PubMed with the help of the combination of different keywords: "Benzothiazole," "antimicrobial activity, anticancer, anti-diabetic, anthelmintic activity." The search was customized by applying the appropriate filters to get the most relevant articles to meet the objective of this review article. There is a various number of research and review article present of benzothiazole derivative in case of different disease which concluded that the benzothiazole is one of the most important scaffolds for the treatment of various disease.

47 illus, 67 ref

001464   SINGH V K, PARLE A (Pharmaceutical Chemistry Dep, Delhi Institute of Pharmaceutical Sciences and Research, New Delhi - 110 017, Email: vineetkumarsingh666@gmail.com) : The intriguing benzimidazole: A review. Int J Pharm Sci Res 2019, 10(4), 1540-52.

Benzimidazole is a heterocyclic aromatic organic compound containing nitrogen. This bicyclic compound is formed by the fusion of benzene with imidazole ring. It is a vital Pharmacophore and privileged structure in medicinal chemistry which exhibits various therapeutic activities like antiulcer, antihypertensive, analgesic, antiviral, antifungal, anticancer and antihistaminic. The disease conditions targeted by these activities are discussed. The present article extensively covers various procedures of synthesis of 2-substituted benzimidazole and its analogs by utilizing different catalysts, solvent conditions, reactants and microwave irradiation with the aim to obtain an inexpensive, ecofriendly, less time-consuming procedure which ensures good yield and quick isolation of the pure product. Ongoing clinical trials of different benzimidazole derivatives exploring additional pharmacological activities are also covered.

5 tables, 85 ref

001392   AUTI P, GABHE S, MAHADIK K (Pharmaceutical Chemistry Dep, Bharati Vidyapeeth Univ, Pune - 411 038, Email: satishgabhe@gmail.com) : Pharmacokinetic studies of secnidazole in the presence of piperine and its synthetic derivative. Int J Pharm Sci Res 2019, 10(3), 1455-61.

Piperine has been widely used as a bioenhancer. Secnidazole is a long-acting 5-nitroimidazole analog. It is used in the treatment of amoebiasis, giardiasis, trichomoniasis and anaerobic bacterial infection. In this study derivative of piperine was synthesized and studied for its bio enhancing the effect and this effect was compared with the bioenhancing effect of piperine. The pharmacokinetic profile of Secnidazole alone and in combination with piperine and piperine derivative was investigated by validated bioanalytical HPLC method as per USFDA guidelines. It was observed that the synthesized derivative of piperine significantly improved the bioavailability of Secnidazole compared to piperine alone in Wistar rats. The N,N-diallyl-5-(benz)(1,3)dioxol5-yl)penta-2,4-dienamide (DA) derivative showed 1.49 fold increase in the bioavailability of Secnidazole. After oral administration of Secnidazole alone and in combination with piperine and piperine derivative (0.035 mmol, 10 mg/kg) there was a significant increase in AUC and C_max of Secnidazole.

7 illus, 5 tables, 22 ref

001390   ARUMUGAM R, PERIAKARUPPAN P (Chemistry Dep, Thiagarajar Coll, Madurai - 625 009, Tamil Nadu, Email: kmpprakash@gmail.com) : Highly selective and sensitive determination of Cr⁶⁺ (nM) in gelatin capsule using AgF/Ag₂WO₄ nanocomposite. Int J Pharm Sci Res 2019, 10(3), 1439-47.

The present work deals with a novel synthesis of AgF/Ag₂WO₄ nanocomposite by co-precipitation method. The morphology and size of the synthesized AgF/Ag₂WO₄ nanocomposite were confirmed by Ultraviolet-Visible (UV-Vis) spectroscopy, Fourier Transform-Infrared (FT-IR) spectroscopy, Transition Electron Microscopy (TEM) and X-Ray Diffraction (XRD) analyses. The performance of the nanocomposite was successfully evaluated for Cr⁶⁺ detection in a gelatin capsule, which indicated that this convenient and sensitive material offered great promise for onsite environmental monitoring of Cr⁶⁺. Control experiments with the addition of over 10 other metal ions (Na⁺ , K⁺ , Mg²⁺, Fe²⁺, Hg²⁺, Ca²⁺, Cu²⁺, Ni²⁺, Mn²⁺ , Zn²⁺) did not result in a distinct change in the colour or in the spectrum of the suspension which indicated that these ions did not interfere in the colorimetric determination of Cr⁶⁺ in gelatin capsule. The detection concentration of Cr (VI) ranged from 0.5 mg to 1.0 mg, and the detection limit was 2 nM.

10 illus, 1 table, 47 ref

001394   BANA A, SATHE M A, RAJPUT S J (The Maharaja Sayajirao Univ of Baroda, Vadodara - 390 002, Email: arpitbana94321@gmail.com) : Analytical method development and validation for simultaneous estimation of halobetasol propionate and mupirocin in the ratio 1:40 by U.V. spectroscopy and RP-HPLC method. Int J Pharm Sci Res 2019, 10(3), 1392-401.

The present work encompasses the development of two classical UV spectroscopy methods and an RP-HPLC method for the concurrent assessment of Halobetasol propionate and Mupirocin inculcating a statistical approach. The UV spectroscopy methods developed herein include absorption ratio method and first derivative spectroscopy method. The wavelength maxima selected for Absorption ratio method were 240 and 220 nm for Halobetasol Propionate and Mupirocin respectively. The zero crossing points selected were 240.626 nm and 220.180 nm for Halobetasol Propionate and Mupirocin respectively for first derivative spectroscopy. The chromatographic separation was achieved by using CHROMBUDGET C18 (250 × 4.6 mm) 5 µm column, mobile phase consisting of Acetonitrile: phosphate buffer (65:35 v/v, pH 3.2), at 1 ml/min flow rate and detection wavelength was 230 nm The retention time of Halobetasol propionate, and Mupirocin was found to be 8.647 ± 0.06 min and 3.357 ± 0.123 min, respectively. Linearity was observed in the concentration range of 5.125 - 5.75 µg/ml for Halobetasol propionate and 5-30 µg/ml for Mupirocin respectively. The analytical method was validated as per ICH, Q2 (R1) guidelines. The developed method was simple, specific and economic, which can be used for simultaneous estimation of Halobetasol propionate and Mupirocin in the gel dosage form.

16 illus, 17 tables, 10 ref

001416   HAQUE M A, BAKSHI V, BOGGULA N, DANDAMUDI S P (Pharmaceutical Chemistry Dep, Anurag Group of Institutions, Ghatkesar - 500 088, Email: narender.b987@gmail.com) : Method development and validations of apixaban in bulk and its formulations by UV-spectroscopy (area under curve). Int J Pharm Sci Res 2019, 10(3), 1387-91.

The aim of the present research work is to validate the apixaban content in bulk and pharmaceutical dosage formulation and validate it as per ICH guidelines. A simple, rapid, precise and highly selective spectrophotometric method was developed for estimation of apixaban in tablet dosage form by the area under curve method. The area under curve method involves the measurement of absorbances of apixaban at the wavelength of 269 nm-289 nm. Methanol was used as a solvent. Linearity was observed in the concentration range of 5-25 µg/ml for apixaban. The accuracy of the method was confirmed by recovery studies of tablet dosage forms and was found to be 100 % for Apixaban. The method showed good reproducibility and recovery with % RSD less than 0.988 %. The LOD of apixaban was found to be 0.335 µg/ml, and LOQ of apixaban was found to be 1.015 µg/ml. Thus the proposed method was found to be rapid, specific, precise, accurate and cost-effective quality control tool for the routine analysis of Apixaban in bulk and tablet dosage form. Drug stability studies have been determined for the formulation under specified conditions, and it was found stable.

2 illus, 6 tables, 18 ref

001483   VANAPATLA S R, BEGAM F (Pharmacognosy and Phytochemistry Dep, Kakatiya Univ, Warangal - 506 009, Email: swarooparanivanapatla@gmail.com) : Evaluation of α-amylase and α-glucosidase enzyme inhibitory activities of Trichuriella monsoniae bennet. Int J Pharm Sci Res 2019, 10(3), 1342-6.

Diabetes is a noncommunicable chronic metabolic disorder characterized by high blood glucose level in the body. One of the antidiabetic therapeutic strategies is the inhibition of carbohydrate-digesting enzymes such as αamylase and α-glucosidase. In the present study methanolic extract and its two fractions (Ethyl acetate and n-butanol) of the whole plant of Trichuriella monsoniae were evaluated for their effect on α-amylase and α-glucosidase enzymes by using invitro assays. The plant extracts were used at varying concentrations to ensure which concentration of the extract/fractions of the plant causes the most inhibition. Phytochemical analysis of the extract and its fractions indicated the presence of flavonoids, steroids/terpenoids, carbohydrates, saponin, phenolic compounds. While tannins and alkaloids are absent. n-butanol fraction shown the prominent α-amylase and α-glucosidase enzyme inhibitory activities (IC₅₀ 4.09 mg/ml and 3.30 mg/ml respectively) than methanolic extract and its ethyl acetate fraction, and it was well comparable with the standard drug acarbose (for α-amylase IC₅₀ 3.62 mg/ml and for α-glucosidase IC₅₀ 2.19 mg/ml). Further, the Total phenolic and flavonoid contents were estimated. These results suggest that Trichuriella monsoniae with a great potential to control postprandial hyperglycemia might be a novel resource for the management of type 2 diabetes.

2 illus, 2 tables, 10 ref

001435   MAHOOD A M, ALKHAFAJI S L (Pharmaceutical Chemistry Dep, Kerbala Univ, Karbala, Iraq, Email: sura.l@uokerbala.edu.iq) : Spectrophotometric determination of etodolac using charge transfer complex. Int J Pharm Sci Res 2019, 10(3), 1330-5.

In this study, we developed a cheap and precise analytic method to measure Etodolac concentration in bulk and pharmaceutical formula. The modified, updated method depends on the reaction between ferric ion and Etodolac to yield ferrous ion. Then the former ion reacted with potassium ferric cyanide to form colored compound has a maximum absorbance at 700 nm. The method was validated by calculating the precision and accuracy. The method follows Beer-Lamber law so that we used the range between 1-22.5 µg/mL and the correlation coefficient at 0.997. Accuracy and precision of the proposed method were estimated and shown average of recoveries between (96.67-99.0 %) with precision represented by RSD % equal to 1.02. We also calculated the detection limit (LOD) and quantitative limit (LOQ), which respectively were 0.6 µg/mL and 1.2 µg/mL. The modified suggested method was used to measure Etodolac in pharmaceutical preparation without drug additives interference and shows a good agreement with the standard method. Therefore, it can be used for routine works for quality control for the estimation of the Etodolac in bulk and pharmaceutical preparation as tablets.

6 illus, 5 tables, 33 ref

001391   ASHANI U B, HARISHA C R, SHUKLA V J (Pharmacognosy Lab Dep, Gujarat Ayurved Univ, Jamnagar - 361 008, Gujarat, Email: urviashani@gmail.com) : Scientific evaluation of Valli panchmoola – different compositions through pharmacognostical and phytochemical methodology. Int J Pharm Sci Res 2019, 10(3), 1325-9.

This study aimed at ensuring the different compositions of Valli panchmoola using authentic herbs and establishing pharmacognostical, physicochemical, and phytochemical standards for the compositions. Compositions of Vallli panchmoola were prepared as per the formula and procedure mentioned in traditional texts and Ayurvedic Formulary of India. The prepared compositions were evaluated for pharmacognostical, physicochemical, and phytochemical parameters using guidelines of the World Health Organization and Pharmacopoeial Laboratory for Indian Medicines for quality control of herbal drugs. Microscopic studies revealed the presence of collenchyma cells, rosette crystals, compound starch grains, parenchyma cells, cluster crystal, etc. Loss on drying 0.17 ± 0.01 %, total ash 1.87 ± 0.02 %, etc. were observed in the classical group. Whereas loss on drying 0.10 ± 0.04 %, total ash 1.77 ± 0.02 %, etc. were observed in group-1. Preliminary phytochemical screening confirms the presence of alkaloids, flavonoids, glycosides, fatty acids, terpenoids, sterols, tannins, proteins, and phenolic compounds. The various pharmacognostical, physicochemical, and phytochemical standards will help in quality control/quality assurance and maintaining batch to batch consistency in herbal drug industries so that maximum therapeutic efficacy can be achieved.

2 illus, 3 tables, 16 ref

001425   KADAM P V, YADAV K N, BHINGARE C L, PATIL M J (Marathwada Mitramandal’s Coll of Pharmacy, Pune - 411 033, Email: kadamprasadv@gmail.com) : Development and validation of a HPLC analytical method for determination of ellagic acid in Epilobium angustifolium extract. Int J Pharm Sci Res 2019, 10(3), 1300-6.

Development of quality assessment parameters for natural products is a prominence necessity to justify their acceptability and activity. Establishment of authentic and reliable analytical methods which profile the quantitative phytochemical composition of marker constituents in multicomponent composition like extract is a challenging task. A simple, rapid, precise, and reliable HPLC method was developed for the separation and estimation of ellagic acid from Epilobium angustifolium (Canadian willow herb) extract. The estimation was carried out using Sunfire C18 column, 5μ (4.6 × 250 mm); mobile phase consisting of 0.1 % orthophosphoric acid and acetonitrile; the flow rate of 1 mL/min and ultraviolet detection at 280 nm with a properly resolved having run time of 35 min. The method was validated as a final verification of method development concerning precision, linearity, accuracy, ruggedness, and robustness. The correlation coefficient (r² ) > 0.999, a method is considered to be linear as the correlation coefficient was found to be within acceptance criteria. The % RSD of peak area response due to ellagic acid in five replicate injections of standard solution was to be less than 2.0 %, and system suitability parameters were passed. The % Average recovery of ellagic acid in Canadian willow Extract observed within the acceptance criterion of 98 - 102 % indicates the accuracy of the method. The present validation proves that the HPLC-method is suitable for the determination of assay of ellagic acid from Canadian willow herb, extract at prescribed conditions.

4 illus, 11 tables, 11 ref

001414   GUNDALA A, KAMMURI D S, CHENGALVA P (Pharmaceutical Analysis and Quality Assurance Dep, Krishna Teja Pharmacy Coll, Tirupati - 517 506, Email: garuna.mpharm@gmail.com) : A novel RP-HPLC method for simultaneous determination of dicyclomine and ethyl morphine in bulk and pharmaceutical formulation. Int J Pharm Sci Res 2019, 10(3), 1229-34.

The present study was designed to develop and validate a simple, sensitive, precise and accurate RP-HPLC method for simultaneous estimation of dicyclomine and ethylmorphine in bulk and tablet dosage form. The chromatographic separation was achieved on Discovery C₁₈ column (250 × 4.6 mm, 5 µm) as stationary phase with a mobile phase of water (pH 5.4 adjusted with orthophosphoric acid): acetonitrile (40:60 v/v) at a flow rate of 1 ml/min and PDA detection at 215 nm. The proposed method was validated for system suitability, specificity, linearity, accuracy, precision, LOD, LOQ, and robustness as per ICH guidelines. The retention times of dicyclomine and ethylmorphine were found to be 3.166 ± 0.02 and 4.204 ± 0.19 min respectively. The calibration curves were linear in the concentration range of 50 % to 150 % of the working concentration (r² =0.999) for both the drugs in a binary mixture. The accuracy was found to be 98.61 % and 99.24 % for dicyclomine and ethylmorphine respectively. The LOD was found to be 0.05 µg/ml, and 0.20 µg/ml and LOQ were found to be 0.17 µg/ml and 0.62 µg/ml for dicyclomine and ethylmorphine respectively. The percentage recoveries for both drugs were in the range of 98-101 %. Hence the proposed RP-HPLC method can be used in routine analysis of tablets containing dicyclomine and ethylmorphine.

8 illus, 7 tables, 11 ref

001420   IDREES M, KOLA S, SIDDIQUI N J (Chemistry Dep, Government Institute of Science, Nagpur - 440 001, Email: idreesshaikh.2009@gmail.com) : An efficient synthesis of some novel bioactive azetidinone derivatives including 5-(benzofuran-2-yl) and 1-phenyl-1h-pyrazole-3-carboxamide moiety. Int J Pharm Sci Res 2019, 10(3), 1214-22.

In continuation of our efforts in the development of novel drugs, in the present article we have described synthesis of a series of novel azetidinones derivatives (4a-i) containing 5-(benzofuran-2-yl) and 1-phenyl-1Hpyrazole-3-carboxamide moiety, with excellent yields and without formation of undesirable side products from cyclo condensation reaction of N'- (benzylidene) -5- (benzofuran- 2- yl) -1 -phenyl -1H -pyrazole- 3-carbohydrazide derivatives (3a-i) with chloro acetyl chloride in the presence of triethylamine in DMF. Carbohydrazones of aryl aldehydes (3a-i) used as the starting compound was obtained by one-pot condensation of 5-(benzofuran-2-yl)-1-phenyl-1H-pyrazole3-carbohydrazide (1) with various substituted aromatic aldehydes (2a-i) and a catalytic amount of acetic acid in ethanol. The structures of newly synthesized compounds have been established through elemental analysis and spectral studies like IR, ¹H NMR, ¹³C-NMR and Mass spectra. All the synthesized compounds were screened for their in-vitro antibacterial activity against different strains of microbes such as S. aureus, E. coli, P. vulgaris and S. typhi at different concentration. The result of the bioactivity confirmed that most of the newly synthesized compounds showed the significant activity when compared with the standard drug Chloramphenicol which might be due to the cyclic carbonyl group present in azetidinones.

1 illus, 2 tables, 23 ref

001424   JAYA S, SRILAXMI G (Pharmaceutics Dep, Anurag Pharmacy Coll, Kodad, Suryapet - 508 206, Email: jayamay24@gmail.com) : Formulation and in-vitro characterization of ambroxol hydrochloride sustained-release matrix tablets. Int J Pharm Sci Res 2019, 10(3), 1208-13.

The present study involves the formulation and in-vitro characterization of sustained release matrix tablets of Ambroxol hydrochloride, a potent mucolytic agent used in the treatment of respiratory disorders. FTIR analysis confirmed the absence of drugpolymer interactions. Sustained release matrix tablets containing 75 mg were formulated employing HPMCK15 and xanthan gum as release retarding polymer and dicalcium phosphate and microcrystalline cellulose as diluents. The powder blend was evaluated for micromeritic properties. The matrix tablets were prepared by direct compression technique. The prepared tablets were evaluated for uniformity of weight, hardness, friability, and uniformity of content. All the formulations showed compliance with pharmacopoeial standards. The in-vitro drug release studies were carried out for a period of 12 h using USP type II dissolution apparatus at 50 rpm by taking 900 ml of 0.1 N HCl (pH 1.2) as dissolution medium for first 2 h and later replacing it with 900 ml pH 6.8 phosphate buffer solution for a period of 10 h at 37 ± 0.5 °C. Among the different combinations of polymers in different ratios studied, the desired in-vitro drug release (97.65 % for 12 h) was found with the combination of HPMC K15M and xanthan gum with the drug in the ratio of 1: 0.75 (F7). The drug release from the F7 formulation followed zero order kinetics and mechanism was found to be erosion.

5 illus, 3 tables, 11 ref

001445   MUNEESWARI P, BHASKARAN S K, POORNIMA K (Biochemistry Dep, Karpagam Academy of Higher Education, Coimbatore - 641 021, Email: poorniovya@gmail.com) : Identification of active pharmaceuticals of Sida acuta Burm. f. leaves using GC-MS and HPTLC fingerprinting. Int J Pharm Sci Res 2019, 10(3), 1194-207.

Sida acuta is one of the medically active plants used for the treatment of multifaceted diseases. However, an elaborated investigation on the phytochemical composition of the ethanolic extract of the leaves of this plant is yet to be deciphered. So, in this quantification of phytochemicals, in-vitro free radical scavenging activity, enzymatic and non-enzymatic antioxidant levels in the fresh leaves, HPTLC fingerprinting and GC-MS analysis in the ethanolic extract of Sida acuta leaves were done. In-vitro antioxidant activities were assayed using DPPH, ABTS, nitric oxide, hydroxyl radical and ferric ions, while ascorbic acid is used as the standard. The results indicated the presence of flavonoids, tannins, phenols, and alkaloids in a reasonably good amount which has substantiated the results of HPTLC. All the tested antioxidants were present prominently in the leaves, specifically catalase and glutathione peroxidase, which may be responsible for the prominent radical scavenging tendency of the extract against the tested free radicals. The GC-MS analysis observed the presence of 35 different compounds each belonging to different classes such as sterols, flavonoids, terpenes, heterocyclic aromatic compounds, phenols, fatty acids, vitamins, alkaloids, and sesquiterpenoids. The results indicate that the ethanolic extract of Sida acuta leaves collected from the Tuticorin District of Tamil Nadu is an effective scavenger of free radicals and has the potential to be used as a natural antioxidant which is attributable to the rich presence of its secondary metabolites.

16 illus, 9 tables, 48 ref

001386   AGARWAL B A, GANDHI S V (Pharmaceutical Chemistry Dep, A.I.S.S.M.S Coll of Pharmacy, Pune - 411 001, Email: babita_a_agarwal@yahoo.co.in) : Study of forced degradation behaviour of a novel proteasome inhibiting anticancer drug by LC-MS and development of a validated stability-indicating assay method. Int J Pharm Sci Res 2019, 10(3), 1186-93.

In the present study, comprehensive stress testing of Carfilzomib, a newly approved proteasome-inhibiting anticancer drug was carried out according to ICH guideline Q1A (R2). The drug was subjected to acid (0.1N HCl), neutral and alkaline (0.1N NaOH) hydrolytic conditions at 70 ºC, as well as to oxidative decomposition at room temperature. Photolysis was carried out in 0.1N HCl, water and 0.1N NaOH at 40 ºC. LC-PDA and LC-MS investigated the products formed under different stress conditions. The LC-PDA method that could separate all degradation products formed under various stress conditions involved a C18 column and a mobile phase comprising of ACN and phosphate buffer (pH 3). The flow rate and detection wavelengths were 1 ml/min and 220 nm, respectively. The developed method was found to be precise, accurate, specific and selective. It was suitably modified for LCMS studies by replacing phosphate buffer with water, where pH was adjusted to 3.0 with formic acid. The drug showed instability in the solution state (under acidic, neutral, alkaline and oxidative stress conditions), but was relatively stable in the solid-state, except the formation of minor products under accelerated conditions. Primarily, maximum degradation products were formed in acid conditions, though the same were also produced variably under other stress conditions. LCMS fragmentation studies characterized the products. Based on the results, a complete degradation pathway for the drug could be proposed. LC-ESI-MS/MS characterized the major stress degradation product, and its fragmentation pathway was proposed.

6 illus, 5 tables, 14 ref

001397   BUDUMURU P, GOLAGANI S, PUSHPANJALI B (Chemistry Dep, GITAM Deemed To Be Univ, Visakhapatnam - 530 045, Email: pushpalatha.budumuru@gmail.com) : Microwave-assisted synthesis of imidazo[1,2-a]pyridine derivatives and their anti-inflammatory activity. Int J Pharm Sci Res 2019, 10(3), 1172-9.

A series of novel Imidazo[1,2-a]pyridine derivatives were synthesized in satisfactory yield by microwave assisted synthetic method. The structures of the newly synthesized compounds are characterized by ¹H-nuclear magnetic resonance (NMR), Fourier transformed infrared (FTIR), mass spectral analysis (LC-MS) and screened for their in-vitro anti-inflammatory activity. Among the synthesized compounds N-(3,5-bis(trifluoromethyl)benzyl)-4-((2-(6- methyl-2-(p-tolyl)imidazo [1,2-a] pyridine-3-yl) acetamido) methyl) benzamide and N- (4-methoxybenzyl)-4- ((2-(6-methyl-2-(p-tolyl) imidazo [1,2-a]pyridin-3-yl) acetamido) methyl) benzamide are possessing high anti-inflammatory activity against standard drug Aspirin. A majority of the tested compounds had shown good consequence to moderate anti-inflammatory activity.

1 illus, 1 table, 25 ref

001436   MAJEED A, RAZA S N, KHAN N A (Pharmaceutical Sciences Dep, Kashmir Univ, Srinagar - 190 006, Email: asmatmajeed4@gmail.com) : Hydrotrophy: Novel solubility enhancement technique: A review. Int J Pharm Sci Res 2019, 10(3), 1025-36.

Drug discovery and development plays a major role in the world and serves mankind. The major criteria to be considered and given importance in drug development is the solubility of a drug. Among all newly discovered chemical entities, about 40 % of drugs fail to reach the market due to their poor aqueous solubility or lipophilicity. Poor solubility is not only a problem for formulation development and clinical testing but also an obstacle at the very beginning while screening new compounds for pharmacological activity. Nowadays oral route is considered as the preferred route of drug administration than other routes due to its convenience in terms of ease of administration and economy. The first requirement of drug which is supposed to be given by oral route is good aqueous solubility, as the poor solubility leads to low absorption, inadequate and variable bioavailability and also gastrointestinal mucosal toxicity. To prevent these crisis, several solubility enhancement techniques have been employed to enhance the solubility of poorly soluble drugs and hydrotropic solubilization is one of them. Besides, the advantage of certain properties like high selectivity, non-inflammability, environmentally friendly, easy availability and cost-effectiveness of hydrotropes makes this technique superior to other solubilization techniques. In the present review, an attempt has been made to discuss the hydrotropic solubilization technique and highlight the applications with this approach.

4 illus, 4 tables, 94 ref

001443   MOLLY B A, PRASANTHI N L (Acharya Nagarjuna Univ, Guntur - 522510, Email: aubinemolly.b@gmail.com) : Cubic liquid crystalline nanoparticles (cubosomes): A novel carrier for drug delivery. Int J Pharm Sci Res 2019, 10(3), 973-84.

Lyotropic liquid crystalline systems, such as reversed bicontinuous cubic phases acquire progressive attention because of their unique microstructure and physicochemical properties. Cubosomes were nanostructured liquid crystalline particles, formed from a certain group amphiphilic lipids in definite proportions in water and was stabilized with a triblock copolymer. Substances in use were biocompatible. Cubosomes are curved bicontinuous lipid bi-layers which were organized in threedimensional structures resembling honeycomb-like structure with distinct amphiphilic, hydrophilic and hydrophobic regions. They serve as a carrier in drug delivery for various bioactive molecules such as chemicals, drugs, peptides, and proteins to protect them from hydrolysis, oxidation or any other way of degradation. Furthermore, several studies have demonstrated the benefits of cubosomes in nanoparticle drug delivery, sustained release, controlled release, and also to provide improved bioavailability. This article gives an overview of initial work that took advancements till drug delivery, cubosomes types, structure, methods of preparation and primarily the applications of cubosomes in the formulation from the past in various categories drugs and pharmaceuticals.

9 illus, 98 ref

001441   MOGHADAS S, MAGHSOUDIPOUR A, EBADZADEH T, ALIZADEH M (Ceramic Div, Materials and Energy Research Centre, Karaj, Iran, Email: s17.moghadas@gmail.com) : Dip-coating of 8YSZ nanocrystalline particles on NiO–YSZ substrate. Bull Mater Sci 2019, 42(2), 84.

In this study, 8 mol % yttria-stabilized zirconia (8YSZ)-agglomerated particles were dispersed in de-ionized water using different weights of Tiron. The results of viscosity and sedimentation measurements of each suspension were evaluated and the optimum amount of Tiron was selected. The most stable suspension was prepared for dip-coating. The substrate was prepared by mixing NiO and YSZ powders and then pressed and pre-sintered at 1050^◦C. The effect of saturated and unsaturated substrates on morphology and thickness of films were investigated. The thickness of YSZ films with different withdrawn speeds and dip-times were calculated. Also, the morphologies of deposited films were characterized by scanning electron microscopy. The above experimental results showed that by adjusting pH about 10, the view point of rheological behaviour, the optimum dispersant was 0.8 % and the suspension containing 0.8 % Tiron had the lowest viscosity. Finally, the obtained layers from dip-coating method represented that the films deposited on saturated substrate were crack-free and homogeneous when compared to unsaturated substrates.

13 illus, 1 table, 19 ref

001444   MULANI K, PATIL V, CHAVAN N, DONDE K (Chemistry Dep, Ramnarain Ruia Coll, Mumbai - 400 019, Email: nitudonde@yahoo.co.in) : Adsorptive removal of strontium(II) using macroporous poly(AGE-co-EGDMA) beads modified with resorcin[4]arene. Bull Mater Sci 2019, 42(2), 82.

Adsorption behaviour of strontium(II) on macroporous poly(allyl glycidyl methacrylate-co-ethylene glycol dimethacrylate) [poly(AGE-co-EGDMA)] beads modified with resorcin[4]arene was studied using macroporous crosslinked [poly(AGE-co-EGDMA)] beads. The macroporous crosslinked [poly(AGE-co-EGDMA)] beads were synthesized by suspension polymerization techniques, followed by functionalization with amino derivatives of resorcin[4]arene. The poly(AGE-co-EGDMA) beads were characterized by FTIR, ¹H and ¹³C-NMR, elemental analysis and particle-size analysis. The surface morphology of beads was studied by scanning electron microscopy. The functionalized poly(AGE-co-EGDMA) beads were used as adsorbents for strontium removal. The crucial factors including the effect of pH, time, initial concentration of metal ions and adsorbent dose were investigated to optimize the maximum adsorption efficiency of Sr(II). The equilibrium data of strontium(II) ions adsorbed on functionalized poly(AGE-co-EGDMA) beads were analysed by pseudo-first- and pseudo-second-order kinetic models. The pseudo-second-order kinetic model indicated that strontium was adsorbed by chemisorption.

16 illus, 4 tables, 22 ref

001486   WANG W G, LI X Y, LIU T, HAO G L (Yan’an Univ, Yan’an 716000, People’s Republic of China, Email: wwgyadx@126.com) : Study on electrical conductivity and oxygen migration of the oxide-ion conductors Na_0.5Bi_0.5Ti_1-xMg_xO_3-x. Bull Mater Sci 2019, 42(2), 80.

Electrical performance and oxygen relaxation behaviour in Na_0.5Bi_0.5Ti_1−xMg_xO_3−x compounds were investigated. The oxide ion conductivity of Na_0.5Bi_0.5Ti_1−xMg_xO_3−x compounds increased first and then decreased with increasing Mg-doped content. The highest oxide ion conductivity of 4.7 × 10⁻³ S cm⁻¹ at 773 K was observed for the Na_0.5Bi_0.5Ti_0.96Mg_0.04O_2.96 compound. A typical relaxation peak in the Na_0.5Bi_0.5Ti_1−xMg_xO_3−x samples was observed. The activation energy and pre-exponential factors were determined as (1.0 eV, 4.7 × 10⁻¹⁶ s) and (0.94−1.0 eV, 6.8 × 10⁻¹⁴−3.1 × 10⁻¹³ s) from internal friction and dielectric relaxation measurement, respectively. The lower oxide ion conductivity in Na_0.5Bi_0.5Ti_1−xMg_xO_3−x (x = 0.06, 0.08, 0.10) compounds may arise from the lower vacancy mobility. Judging from the electrical performance and relaxation parameters, although lower-level Mgdoping can improve oxide ionic conductor, oxygen vacancy mobility in Na_0.5Bi_0.5Ti_1−xMg_xO_3−x compounds cannot be improved with increasing Mg-doping content. These results will be meaningful to ameliorate the electrical properties of Na_0.5Bi_0.5Ti_1−xMg_xO_3−x compounds and understand the relationship between the electrical properties and structure.

15 illus, 1 table, 26 ref

001423   JAIN P, KAUR M, KAUR M, GREWAL J K (Chemistry Dep, Punjab Agricultural Univ, Ludhiana - 141 004, Email: manmeetgill885@gmail.com) : Comparative studies on spinal ferrite MFe₂O₄ (M = Mg/Co) nanoparticles as potential adsorbents for Pb(II) ions. Bull Mater Sci 2019, 42(2), 77.

Ferrite nanoparticles (NPs) with composition MFe₂O₄ (M = Mg/Co) were synthesized by a facile combustion method. NPs were characterized employing various physico-chemical techniques. X-ray diffraction patterns confirmed the phase purity, transmission electron micrographs indicated that NPs are spherical and average diameter of maximum fraction of NPs was in the range of 20–30 nm. Magnetic studies revealed that the saturation magnetization values for MgFe₂O₄ and CoFe₂O₄ NPs were 13.17 and 41.12 emu g⁻¹, respectively. The Brunauer–Emmett–Teller surface area of CoFe₂O₄ and MgFe₂O₄ NPs was 22.98 and 34.39 m² g⁻¹, respectively. Synthesized ferrite NPs and activated charcoal were comparatively analysed as adsorbents for removal of Pb(II) ions. The factors influencing uptake behaviour of Pb(II) ions viz. adsorbent dose, pH, concentration, temperature and contact time were quantified. The adsorption data showed good correlation with Langmuir and Freundlich models as compared to Dubinin–Radushkevich model. The maximum adsorption capacity displayed a twofold increase for NPs as compared to activated charcoal. The easy magnetic separation of ferrite NPs from the solution and their regeneration with 0.1 N NaOH for reuse without any loss make them potential adsorbents. The trend in ascending order for the elimination of Pb(II) ions from the solution was activated charcoal < CoFe₂O₄ NPs < MgFe₂O₄ NPs. The observed differences in the adsorption potential of NPs are explained on the basis of structural and magnetic properties and the surface area of NPs.

11 illus, 4 tables, 36 ref

001404   DEVI J M (SASTRA Deemed Univ, Thanjavur - 613 401, Email: jmeenadevi@sastra.ac.in) : Simulation of graphene–fullerene nanohybrid structure. Bull Mater Sci 2019, 42(2), 75.

In the present simulation study, the structure and dynamics of graphene–fullerene nanocomposite has been investigated using all atom molecular dynamics simulation technique. The formation of graphene–fullerene nanocomposite constituting graphene and self-assembly of 12 bucky balls has been demonstrated. The structure, size, interparticle separation, spatial distribution, temperature effect, mobility and conformation of graphene–fullerene nanocomposite, and the influence of single and two layers of graphene on the structure of graphene–fullerene nanocomposite have been determined and discussed in detail. This simulation result may possibly aid the design and development of graphene–fullerene hybrid nanomaterials for future biological and technological applications.

12 illus, 5 tables, 56 ref

001417   HASSAN M S, JANA A, GAHLAWAT S, BHANDARY N, BERA S, INGOLE P P, SAPRA S (Chemistry Dep, Indian Institute of Technology Delhi, New Delhi - 110 016, Email: sapra@chemistry.iitd.ac.in) : Colloidally synthesized defect-rich MoSe₂ nanosheets for superior catalytic activity. Bull Mater Sci 2019, 42(2), 74.

Transition metal dichalcogenide (TMD) nanosheets (NSs) with defect-rich and vertically aligned edges are highly advantageous for various catalytic applications. However, colloidal synthesis of defect-rich NSs with thickness variation has been a challenging task. Here, we report a colloidal synthesis of 2H-MoSe₂ NSs having a large number of defects and vertically aligned edges, where the thickness is varied by changing the amount of coordinating solvent. The Se-vacancies in these NSs have introduced defect sites which are corroborated by the presence of additional vibration modes in Raman spectra. These NSs exhibit electrocatalytic hydrogen evolution reaction performances with a low overpotential (210–225 mV) at 10 mA cm⁻² current density and a small Tafel slope (54–68 mV per decade). Moreover, these MoSe₂ NSs are also employed as counter electrodes (CEs) for the fabrication of dye sensitized solar cells via a cost-effective and simplified procedure. The power conversion efficiencies of 7.02 ± 0.18 %, comparable with Pt CE (7.84 ± 0.10 %) could be routinely achieved. These results demonstrate a novel synthetic strategy to prepare layered TMDs with superior catalytic applications.

4 illus, 3 tables, 72 ref