000334   TAYA P, MEHTA D K, DAS R (Pharmaceutical Chemistry Dep, Maharishi Markandeshwar (Deemed to be Univ), Ambala - 133 207, Email: dkmehta17@rediffmail.com) : Design, synthesis, docking study and pharmacological evaluation of novel -2- (5-(1h-indol-3-yl)- 1, 3, 4-thiadiazol -2 -ylimino) -5 -(substituted benzylidene) thiazolidin-4-one analogues. Int J Pharm Sci & Res 2019, 10(2), 701-11.

A series of novel analogues of 2-(5-(1H-indol-3-yl)-1, 3, 4- thiadiazol-2-ylimino)- 5- (substituted benzylidene)thiazolidine-4-one have been synthesized. The structures of newly synthesized compounds were confirmed by FT-IR, ¹H-NMR, ¹³C-NMR and Mass spectroscopy. The synthesized compounds showed significant antibacterial activity against gram-positive bacteria: Staphylococcus aureus (MTCC 3160), Bacillus subtilis (MTCC 2061), gramnegative Escherichia coli (MTCC 1652), Pseudomonas aeruginosa (MTCC 741) and antifungal activity against fungal strains: Candida albicans (MTCC 183) and Aspergillus niger (MTCC 2110). Also, their anti-inflammatory activity was evaluated by using carrageenan-induced rat paw edema method. Compounds 7d and 7h with the methoxy substitution on phenyl ring were found as active derivatives of the series, exhibited 49.86 % and 49.88 % inhibition respectively as compared with Diclofenac sodium. In-silico molecular docking studies of the synthesized compounds was done on crystal structures of proteins of microbes Aspergillus niger, Bacillus subtilis, Candida albicans, Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus and cyclooxygenase-2 using GRIP batch docking method of V-life MDS 3.0 software to study their observed activity which revealed a significant correlation between the binding score and biological activity for these compounds.

3 illus, 6 tables, 25 ref

000326   SUDJARWO, ALFI M N, ANNURYANTI F (Pharmaceutical Chemistry Dep, Airlangga Univ, Surabaya, Indonesia, Email: sudjarwo0958@gmail.com) : Validation and development of TLC-densitometry method for standardization of soursop leaf extract (Annona muricata Linn.) with quercetin. Int J Pharm Sci & Res 2019, 10(2), 686-91.

Standardization is a process involving various chemical analysis methods based on pharmacological data involving general physical and microbiological analyzes aimed at the safety of a natural extract. To obtain the correct result, the standardization step is preceded by method validation. Quercetin can be obtained from the leaves of soursop (Annona muricata Linn.), which use for treatment fever, diarrhea, anti-convulsive, antifungal, antimicrobial, gout, itching, and flu. Determination of quercetin in soursop leaf extract using TLC-Densitometry must be validated by testing selectivity, limit of detection (LOD), limit of quantification (LOQ), linearity, precision, accuracy, and range. Densitometry scanning of the plates silica gel 60 F₂₅₄ directly at 265 nm was used for analysis of quercetin. The result of selectivity test was 1.53 (>1.5) with mobile phase toluene: ethyl acetate: formic acid (4: 3: 0.4; v/v/v), limit of detection (LOD = 0.018 µg), limit of quantification (LOQ = 0.060 µg), linearity y = 9387.3x – 767.39 (r = 0.9996 and Vxo = 1.9 %), Coefficient of Variation (C.V.) of precision 1.906525 % and the percent recovery of 96.6 % ± 8.26 %. The validated and development method was applied for standardization of quercetin in soursop leaf extract and resulted in the quercetin assay in soursop leaf extract was 1.288 % ± 9.996 % (w/w).

3 illus, 3 tables, 35 ref

000206   FALEYE F J, AJAYI C B, AKINWUMI O A, POPOOLA O K (Chemistry Dep, Ekiti State Univ, Ado-Ekiti, Nigeria, Email: fjfaleye2002@yahoo.com) : Evaluation of methanolic extract of Chytranthus macrobotrys seed (CMS) for antimicrobial, α-glucosidase and α-amylase inhibitory activities. Int J Pharm Sci & Res 2019, 10(2), 678-85.

Chytranthus macrobotrys (Sapindaceae) is one of the notable African medicinal plants with traditional history but lack scientific data. This report was aimed to evaluate C. macrobotrys seed (CMS) methanol extract for its phytochemical composition, antimicrobial activity, α-glucosidase, and α-amylase inhibitory activities. Methanolic extract of C. macrobotrys seed was investigated for its chemical composition, antimicrobial activity, α-glucosidase, and α-amylase inhibitory activities. The results revealed the presence of flavonoid (18.61 ± 1.88 mg/100g), phenol (28.71 ± 2.95 mg/100g), tannin (17.29 ± 1.84 mg/100g), terpene (587.07 ± 3.63 mg/100g), sterol (111.54 ± 3.85 mg/100g) and saponin (761.78 ± 1.35 mg/100g). The extract using agar diffusion method showed antimicrobial activity against Staphylococcus aureus, Proteus vulgaris, Pseudomonas aureuginosa, Streptococcus pneumonia, Bacillus cereus, and Micrococcus luteus with a diameter of inhibition zones from 10-20 mm. A weak antimicrobial activity was observed against Escherichia coli and Shigella sp. while no activity was observed against Klebsiella pneumonia and Salmonella typhi. The CMS showed αglucosidase and α-amylase inhibitory activity at the concentration range of 10-100 µg/ml. The highest % inhibition was observed at 100 µg/ml (41.61 ± 1.85) and (37.90 ± 1.89) respectively. The study nominated CMS as a possible alternative natural remedy in the treatment of microbial infections and diabetes. Therefore, elucidating the active components, mechanistic mode of actions and further subjection of CMS for an in-vivo study are required.

2 illus, 3 tables, 31 ref

000324   SUBBIAH M, THENNARASAN S, VAJIRAVELU S (Chemistry Dep, Pachaiyappa’s Coll, Chennai - 600 030, Email: sivaatnus@gmail.com) : Effect of marine brown alga Lobophora variegata (J. V. Lamouroux) Womersley ex E. C. Oliveir various solvents extracts on dermatophytes. Int J Pharm Sci & Res 2019, 10(2), 672-7.

We here in the report the investigation of the antifungal activity of various solvent extracts obtained from a marine brown alga, Lobophora variegata against three fungal dermatophytes, namely Candida albicans, Candida tropicalis, Trichophyton mentagrophytes and a nondermatophyte Aspergillus flavus using disc diffusion method. Among the solvent extracts tested in the investigation, only the methanol extract of the L. variegata exhibited better antifungal activity against all the fungi and chloroform extract was able to elicit activity against C. albicans and T. mentagarophytes. On the other hand, the extract of the L. variegata obtained from ethyl acetate was active against C. albicans only. In contrast to the methanol and chloroform extracts, the aqueous and hexane extracts of the L. variegata were found to be least effective and showed no observable activity against any of the test fungi. The investigation demonstrated that the methanol extract of brown alga L. variegata is more effective on dermatophyte fungi.

2 illus, 2 tables, 25 ref

000251   MAHESHWARI A, LOONKER S (Chemistry Dep, Jai Narain Vyas Univ, Jodhpur - 342 001, Email: maheshwari.akanksha90@gmail.com) : Microwave assisted synthesis, characterization and biological evaluation of newly synthesized 1, 3, 4-thiadiazole derivative of guar gum. Int J Pharm Sci & Res 2019, 10(2), 666-71.

A new derivative of Guar gum, incorporated with 1, 3, 4-thiadiazole nucleus was synthesized by using a new green and efficient synthetic approach. Guar gum is a biodegradable polymer having numerous applications in various industries. Thiadiazole compounds are well known in the therapeutic world due to their pharmacological importance. The newly synthesized derivative was characterized by IR, H¹ NMR, and mass spectrometry. Its antioxidant activity was determined by hydrogen peroxide scavenging activity. Its antimicrobial activity was also studied.

10 illus, 3 tables, 15 ref

000295   RAO P V, RAO A L, PRASAD S V U M (Pharmaceutical Analysis Dep, Vikas Coll of Pharmacy, Vissannapeta - 521 215, Email: venkats0425@gmail.com) : A novel stability indicating RP-HPLC method for simultaneous estimation of anti-viral class of elbasvir and grazoprevir in bulk and pharmaceutical dosage form. Int J Pharm Sci & Res 2019, 10(2), 655-60.

To develop accurate, precise stability indicating a method for simultaneous estimation of Elbasvir and Grazoprevir in bulk and pharmaceutical dosage form. Simple, rapid, precise, sensitive and reproducible validated stability-indicating Reverse-Phase HighPerformance Liquid Chromatography (RP-HPLC) method for the quantitative analysis of Elbasvir and Grazoprevir in the pharmaceutical dosage form. Chromatographic separation was carried out on waters Alliance-2695, by using Luna C18 (150 mm × 4.6 mm, 5 µm) column and the mobile phase containing OPA buffer (0.1 %) and acetonitrile in the ratio of 50:50 v/v. The flow rate was 1.0 ml/min; detection was carried out at 258 nm using a photodiode array detector at ambient temperature. The number of theoretical plates and tailing factor for Elbasvir and Grazoprevir were obtained to be NLT 2000 and should not more than 2 respectively. The linearity of the method was excellent over the concentration range 1.53-22.95 µg/ml and 3.05-45.75 µg/ml for Elbasvir and Grazoprevir respectively. The correlation coefficient was 0.999 %. The relative standard deviation of peak areas of all measurements was less than 2.0. The proposed method was validated according to ICH guidelines. The method was found to be a simple, economical, suitable, precise, accurate and robust method for quantitative analysis of Elbasvir and Grazoprevir in combination and its stability.

5 illus, 5 tables, 9 ref

000283   PRASAD R, BHATT S, SINGH K (Chemistry Dep, SRK Univ, Bhopal - 462 047, Email: ramesh_prasad81@rediffmail.com) : HPLC method for simultaneous estimation of drug release of ledipasvir and sofosbuvir in ledipasvir and sofosbuvir tablets. Int J Pharm Sci & Res 2019, 10(2), 634-41.

Analytical scientists of the pharmaceutical industry aimed at developing robust HPLC methods for analysis of generic drug products. This paper deals with HPLC method of analysis for estimation of % drug release of Ledipasvir and Sofosbuvir in Ledipasvir and Sofosbuvir tablets used for the treatment of chronic hepatitis C virus (HCV) infection. For analysis of dual combination drug product, HPLC method uses ‘Zorbax Eclipse Plus C18 100 × 4.6 mm, 3.5 µm’ HPLC column, a combination of buffer pH 3.0 and acetonitrile as mobile phase in gradient mode with UV detection at 260 nm. The method was validated and found to be precise, robust, accurate and linear (in range 9.05 to 54.3 µg/mL and 2.045 to 12.27 µg/mL of Sofosbuvir and Ledipasvir respectively). The method was also found to be specific for blank and placebo solutions. This ensures suitability of the method for simultaneous quantitative determination of % drug release of Ledipasvir and Sofosbuvir in a pharmaceutical formulation. In the pharmaceutical industry, this method can be used for routine as well as stability samples analysis in formulation product.

4 illus, 14 tables, 12 ref

000179   BEGUM S A, MADHURI V, PADMALATHA K (Pharmaceutics Dep, Chalapathi Institute of Pharmaceutical Sciences, Guntur - 522 034, Email: arifashaik2007@gmail.com) : Design and evaluation of fast dissolving tablets of roflumilast solid dispersions. Int J Pharm Sci & Res 2019, 10(2), 599-611.

The main objective of the present investigation was to formulate and evaluate fast dissolving tablets of Roflumilast solid dispersions using a direct compression method. Roflumilast solid dispersions were prepared by solvent evaporation as well as melting method. Roflumilast is a selective, long-acting inhibitor of the enzyme PDE-4 and has anti-inflammatory effects. It is used orally in the treatment of chronic obstructive pulmonary disease (COPD). The roflumilast drug belongs to BCS class II drugs that have low solubility and high permeability. The current research work was focused on improving the aqueous solubility of Roflumilast using solid dispersion technique and enhancing the dissolution rate. Based on the results of solubility analysis, phosphate buffer pH 6.8 was chosen as the dissolution medium. The powder blend of Roflumilast solid dispersions was evaluated for flow characteristics. The fast dissolving tablets of Roflumilast solid dispersions were subjected to post-compression parameters such as weight variation, hardness, thickness, friability, drug content, wetting time, water absorption ratio, invitro dispersion time and in-vitro disintegration time and the results were found to be within the acceptable limits. Based on FT-IR spectra obtained, it was evident that there was no significant interaction of Roflumilast with carriers and other excipients. From the results of dissolution study, SD1 and SD18 formulations were considered as best formulations.

8 illus, 21 tables, 16 ref

000233   KEMISETTI D (Pharmaceutical Chemistry Dep, Vaagdevi Pharmacy Coll, Warangal - 506 005, Email: kdp251999@gmail.com) : Synthesis of paracetamol-peg prodrugs, in-vitro and in-vivo evaluation. Int J Pharm Sci & Res 2019, 10(2), 578-85.

Paracetamol is a well-known drug for its antipyretic, analgesic and anti-inflammatory activity. The drug being an OTC had been used more frequently than required. As a result of this overdosage of the drug caused a hepatotoxic effect. So to overcome this, an approach of PEGylation was chosen. PEG 1500- Paracetamol, PEG 6000-Paracetamol, PEG 1500-Glycine-Paracetamol, and PEG 6000-Glycine- Paracetamol. The Prodrugs synthesized were subjected to in- vitro dissolution at λ_max 256nm at pH 1.2, 4.5 and 6.8. The studies revealed that % drug release was more at pH 6.8 rather than at pH 1.2 and 4.5, for PEG 6000-GlyParacetamol than PEG 1500-Gly-Paracetamol and also PEG 6000-Paracetamol % drug release was more than PEG 1500-Paracetamol. In-vivo Analgesic activity by Tail Immersion method revealed that PEG 6000-Gly-Paracetamol and PEG 1500- Gly-Paracetamol has higher analgesic activity than PEG-PEG 6000-Paracetamol and PEG 1500-Paracetamol, which indicates the influence of spacer, i.e., Glycine on drug release. In-vivo Analgesic activity by hot plate method and acetic acid methods revealed that PEG 6000-Gly-Paracetamol and PEG 6000-Paracetamol has higher analgesic activity than PEG 1500-Gly-Paracetamol and PEG 1500-Paracetamol, which indicates the influence of higher molecular weight on drug release.

11 illus, 5 tables, 28 ref

000246   KURUVILLA J, IYER R S, ANILKUMAR M (Botany Dep, Union Christian Coll, Ernakulam - 683 102, Email: drmakumar@gmail.com) : Phytochemical evaluation and HPTLC fingerprint profile of Cissus latifolia Lam. stem. Int J Pharm Sci & Res 2019, 10(2), 568-77.

Cissus latifolia Lam. (Vitaceae) is a woody climber with leafopposed tendrils. It is a medicinal plant used in the traditional system of medicine for the treatment of various ailments. The present study focused on the identification and qualitative determination of phytoconstituent types and establishment of the HPTLC fingerprint profile of the hot and cold extracts of C. latifolia. Preliminary phytochemical screening was done to identify the class of compounds present. HPTLC analyses of eight different extracts were carried out with the most suitable mobile phase system using the Camag HPTLC instrument consisting of Linomat- V automated spotter having a 100 μl syringe connected to a nitrogen cylinder, twintrough developing chamber, scanner-III and viewing cabinet with dual wavelength UV lamps (Camag, Muttenz, Switzerland). Qualitative phytochemical screening revealed the presence of flavonoids, coumarins, tannins, alkaloids, steroids, terpenoids, saponins, quinines, anthraquinones and phenol in the stem of C. latifolia. The HPTLC profiling of eight different extracts showed the presence of alkaloids, flavonoids, phenols, saponins, and tannins with different Rf values. The results of preliminary phytochemical screening and HPTLC fingerprint obtained from this study can be used as a reference for the standardization and quality control of Cissus latifolia stem.

5 illus, 6 tables, 23 ref

000279   PAUL B, ADIMOOLAM S, QURESHI M J (Dosage Form Design Dep, MAHSA Univ, Selangor, Malaysia, Email: senthil@mahsa.edu.my) : Formulation and in-vitro evaluation of metronidazole loaded HPMC K15M mucoadhesive microcapsules for H. pylori infection using 3²- full factorial designs. Int J Pharm Sci & Res 2019, 10(2), 555-67.

The purpose of the research was to develop and evaluate metronidazole loaded HPMC K15M mucoadhesive microcapsules for sustained drug release at the gastric mucosa. Metronidazole mucoadhesive microcapsules were formulated by ion gelation technique using 3² factorial designs. A 3² full factorial designs were used to derive a statistical equation, ANOVA analysis, contour plots, and 3D response surface plots. Different polymer ratios of HPMC K15M and sodium alginate were used to formulate nine formulations (F1 to F9) of HPMC K15M loaded mucoadhesive microcapsules of metronidazole. In-vitro drug release and mucoadhesion were carried out by USP29 type-II tablet dissolution test apparatus and disintegration tester using goat stomach mucosa. The formulation was characterized by determining possible drug-polymer interaction using FT- IR, the percentage of yield, particle size, the percentage of entrapment efficiency, swelling index, the percentage of mucoadhesion and percentage of drug release. FT-IR spectroscopy result shows the interaction between the drug and polymers combined. The optimized formulations F9 exhibited high drug entrapment efficiency of 92.07 ± 0.02%, particle size of 852.46 ± 0.04 (μm), percentage yield of 96.36 ± 0.04%, swelling index of 99.25 ± 0.02 %, percentage of mucoadhesion after 8 h was 69.00 ± 0.04 %, and the drug release (49.70 ± 0.01 %) sustained more than 14 h. Metronidazole mucoadhesive microcapsules adhered more strongly to gastric mucous layer and could retain in the gastric mucosa for an extended period, followed by a non-Fickian type of release. The study shows that metronidazole mucoadhesive microcapsules can be effectively used for sustained drug release to the gastric mucosa in the treatment of H. pylori infection.

15 illus, 5 tables, 49 ref

000306   SEEMAISAMY R, FARUCK L H, GATTU S, NEELAMEGAM R, BAKSHI H A, RASHAN L, AL-BULOSHI M, HASSON S S A A, NAGARAJAN K (Zoology Dep, Periyar Univ, Salem - 636 011, Email: kayalvizhinagarajan@gmail.com) : Anti-microbial and anti-cancer activity of Aegle marmelos and gas chromatography coupled spectrometry analysis of their chemical constituents. Int J Pharm Sci & Res 2019, 10(1), 373-80.

In this study, we investigated anti-cancer and antimicrobial activity of Aegle marmelos leaf extracts and their chemical profile characterized by gas chromatography coupled mass spectrometry (GC-MS). A. marmelos leaves were extracted with acetone, methanol, ethanol, and chloroform. Presence of phenolic compounds was identified in these extracts by qualitative analysis. All the extracts were subjected for anti-bacterial activity against the different strains of bacteria (Staphylococcus aureus, Bacillus subtilis, Bacillus cereus, Bacillus ariyabattai, Bacillus megaterium, Pseudomonas putida, Klebsiella pneumonia, Serratia marcescens, and Escherichia coli). It is noteworthy that acetone extract elicited maximum growth inhibition on Serratia marcescens. Based on profound anti bacterial activity, acetone and methanol extract of A. marmelos were checked for cytotoxicity against MDA-MB-231, HEp-2 and vero cells. MDA-MB-231 cells were more sensitive to acetone extract of A. marmelos with an IC₅₀ value of 79.62 µg/ml where as HEp-2 cells are more sensitive to methanol extract of A. marmelos with an IC₅₀ value of 47.08 µg/ml. Vero cells withstand 24 h treatment of both extract, and it is evidenced that both acetone and methanol extract of A. marmelos exhibited chemo sensitive property towards cancer cells. GCMS analysis was performed to characterize the active principles of acetone and methanol extracts of A. marmelos. GC MS data revealed the presence of ten major components. Overall, both acetone and methanol extract of A. marmelos found to be promising anti antibacterial and anti-cancer agent however the active principle of these should be isolated and characterized before reaching a concrete scientific conclusion.

6 illus, 3 tables, 14 ref

000316   SINGH K, BHATT S, PRASAD R (Chemistry Dep, Sarvepalli Radhakrishnan Univ, Bhopal - 462 026, Email: kaushlendra0707@gmail.com) : HPLC method for estimation of drug release of sofosbuvir in pharmaceutical formulation. Int J Pharm Sci & Res 2019, 10(1), 367-72.

Pharmaceutical industry and quality control laboratories needs of robust methods for analysis of drugs used in the treatment of lifethreatening diseases such as hepatitis C. Using HPLC technique, a rapid, selective, precise and accurate method was developed and validated for the estimation of % drug release of Sofosbuvir in a pharmaceutical formulation. Stability indicating HPLC method was developed using Zorbax eclipse plus C18 (100 × 4.6 mm), 3.5 µ as analytical column and a combination of ammonium acetate buffer pH 5.3 and methanol in the ratio (45: 55) was used as mobile phase in isocratic mode. UV detection was carried out at 260 nm, column temperature was maintained at 25 °C, and the flow rate was 1.5 ml/min. The method was validated as per internationally accepted ICH guideline and found to be specific for blank and placebo solution, precise, robust, accurate and linear in range 9.2 to 69.0 µg/ml of Sofosbuvir. This method can be used for routine analysis of pharmaceutical formulation in any quality control laboratory leading to delivery of good quality healthcare solution.

4 illus, 11 tables, 9 ref

000213   GOSWAMI J A, SHAH N J (Quality Assurance Dep, RK Univ, Rajkot - 360 020, Email: jigargoswami013@gmail.com) : Stability indicating RP-HPLC method for combination of ambroxol hydrochloride and levofloxacin hemihydrate in pharmaceutical formulation. Int J Pharm Sci & Res 2019, 10(1), 356-62.

Ambroxol hydrochloride (AMB) and Levofloxacin hemihydrate (LVF) in combination were separated using Reverse-Phase - High-Performance Liquid Chromatographic (RP-HPLC) method. Mobile phase acetonitrile and 0.05 M potassium di-hydrogen orthophosphate buffer (pH 7.0 adjusted with sodium hydroxide solution) (50: 50, v/v) was selected for this chromatographic method. The separation was achieved in Zorbax Eclipse XDB -C18 column with (250 × 4.5 mm i.d), 5$\mathrm{\mu }$m particle size with a flow rate of 1.0 ml/min. At 248 nm wavelength, 10 µl of 60 µg/ml Ambroxol hydrochloride and 400 µg/ml Levofloxacin hemihydrate (LVF) was injected for 15 min runtime, and an individual peak was obtained for LVF at retention time 2.61 min and for AMB at retention time 7.69 min. Linearity was achieved for Ambroxol hydrochloride in the range of 48 mcg/ml to 72 mcg/ml and Levofloxacin hemihydrate in the range of 320 mcg/ml to 480 mcg/ml. For stress degradation, AMB and LVF were subjected to acid hydrolysis, base hydrolysis, thermal degradation, UV light degradation, oxidation and analyzed with this chromatographic method. The results obtained with this method are useful for assay of this pharmaceutical formulation; hence this method can be used in the pharmaceutical industry.

10 illus, 10 tables, 7 ref

000269   NITHYA V, KAMALAM M (Botany Dep, PSGR Krishnammal Coll for Women, Coimbatore - 641 004, Email: kamaluma12@gmail.com) : Estimation of quercetin content in three different species of eupatorium by high-performance thin-layer chromatography. Int J Pharm Sci & Res 2019, 10(1), 303-08.

Three different species of Eupatorium namely E. glandulosum, E. odoratum and E. triplinerve belongs to the family Asteraceae are selected for the analysis of quercetin content. Leaves are extracted with ethanol and water and used for the analysis of quercetin by HPTLC technique using the mobile phase containing toluene: ethyl acetate: formic acid: methanol (5.5:4:1:0.5). Determination of quercetin content was performed by densitometric scanning under 254 nm, and the quercetin was detected at the R_f value of 0.54. The quantity of the quercetin content in plant extract was estimated by the calibration curve obtained from the standard quercetin. The result showed that the ethanolic extracts of E. glandulosum showed a high amount of quercetin (17.44 mg/g) followed by E. odoratum (13.4 mg/g) and E. triplinrve (9.29 mg/g).

10 illus, 2 tables, 20 ref

000182   BHATTACHARYYA S, SOGALI B S (Pharmaceutics Dep, Krupanidhi Coll of Pharmacy, Bangalore - 560 035, Email: sayanibh@gmail.com) : Validation for quantitative determination of aztreonam in simulated lung fluid by UV spectroscopy method. Int J Pharm Sci & Res 2019, 10(1), 222-26.

Aztreonam, a synthetic beta-lactam antibiotic is widely used for the treatment of infections in lungs, meninges, bladder, etc. Its potential use in the treatment of pneumonia and cystic fibrosis has been established. Recently FDA has approved Cayston® for inhalation therapy of Aztreonam in lungs infection. Many studies have been reported on the quantitative determination of Aztreonam by UV spectrophotometric and HPLC method. The present study focuses on the quantitative spectrophotometric determination of Aztreonam in two simulated lungs fluid namely artificial lysosomal fluid (ALF) and gamble solution. The λ_max was found at a wavelength of 293 nm for both the solutions. Further, the method developed was validated for its linearity, precision by interday and within day study, accuracy, specificity, robustness and determination of limit of quantification and limit of detection in both the solutions. The linearity demonstrated a correlation coefficient of 0.9995 and 0.9999 in ALF and gamble solution respectively. The LOD was found to be 0.38 µg/ml and 0.18 µg/ml for ALF and gamble solution respectively. The LOQ was found to be 1.15 µg/ml and 0.53 µg/ml for ALF and Gamble solution respectively. The proposed method was found to be simple, rapid, accurate, precise, and specific for the determination of Aztreonam in simulated lungs fluid.

5 tables, 14 ref

000255   MATHUR M, DEVI V K (Pharmaceutics Dep, Al-Ameen Coll of Pharmacy, Bangalore - 590 027, Email: aacp112015@gmail.com) : Design of experiment utilization to develop and validate high-performance liquid chromatography technique for estimation of sertaconazole nitrate. Int J Pharm Sci & Res 2019, 10(1), 214-21.

A novel method of estimation and validation of Sertaconazole nitrate (SER) by Reverse Phase-High Performance Liquid Chromatography coupled with Ultra-violet detection was developed which had high potential in determining drug concentration with more precision and high accuracy. The process of elution was conducted using Phenomenex C₁₈ (250 mm × 4.6 mm i.d., 5.0 μm) using 0.01M monobasic sodium phosphate and acetonitrile in a ratio of 28:72 % v/v as mobile phase at 4.5 pH and a flow rate of 1.0 mL/min. Detection was carried out using a UV detector at 260 nm. This precise method was linear between a range of 10 to 500 μg/ml with R² close to one (0.999). The limit of detection (LOD) and limit of quantification (LOQ) of SER was found to be 0.1 μg/ml and 0.15 μg/ml respectively. The method was validated for accuracy, precision, linearity, LOD, LOQ, and robustness. Validation studies demonstrated that this HPLC method is simple, specific, rapid, reliable and reproducible. The 3-level 2-factor facecentred central composite design was employed using Design Expert Software ver. 7.0.0 to examine the effect of independent chromatographic factors like pH of the mobile phase and the ratio between 0.01M monobasic sodium phosphate and acetonitrile on the dependent factors like peak area, theoretical plates and tailing factor. The ANOVA studies proved that the model employed for this study was significant. This method can be used as a more convenient and efficient option for the analysis of SER to establish the quality of the drug substance during routine analysis with consistent and reproducible results.

4 illus, 5 tables, 18 ref

000249   MADHAVI K, SWATHI K, ANITHA B, SREE G R U, SRAVANTHI G, ASHWINI G (Pharmaceutical Chemistry Dep, Sri Padmavati Mahila Visvavidyalayam (Women’s Univ), Tirupati - 517 502, Email: kuchanamadhavi@yahoo.co.in) : Synthesis and evaluation of novel α-cyano-n-(4-hydroxyphenyl) cinnamamides for antioxidant, anti-inflammatory activities: In-silico prediction of drug likeness properties. Int J Pharm Sci & Res 2019, 10(1), 203-13.

A facile synthetic reaction has been used for the synthesis of novel compounds, substituted α-cyano-N-(4-hydroxyphenyl) cinnamamides from α-cyano-N-(4-hydroxyphenyl) acetamide. Their physical and spectral data characterized all the synthesized compounds. The title compounds were screened for in-vitro antioxidant activity in two different models which include scavenging of DPPH and nitric oxide free radicals. The compounds with hydroxy substitution on the phenyl ring of α-cyanocinnamamide moiety showed excellent antioxidant properties. Hence, the active compounds were evaluated for anti-inflammatory activity by carrageenan-induced rat paw edema assay. Among the evaluated compounds, α-cyano-N-(4-hydroxyphenyl)-4-hydroxy-3- methoxycinnamamide and α-cyano-N-(4-hydroxyphenyl)-3,4-dihydroxycinnamamide exhibited better activity comparable to the standard drug Diclofenac. Further, in-silico prediction of molecular properties of the synthesized compounds was carried out using molinspiration online software. The study revealed that all the compounds obeyed Lipinski’s rule of five. The TPSA calculations revealed that the compounds possess good intestinal absorption. Finally, the present study identified these compounds as potential new drug candidates for the treatment of diseases associated with oxidative stress.

5 tables, 36 ref

000264   NAKVE A, KHADABADI S S, RAI P D (Ram-Eesh Institute of Vocational and Technical Education, Greater Noida - 201 310, Email: raipallav@gmail.com) : A stability indicating RP-LC method for the determination of strychnine in Krimimudgara rasa. Int J Pharm Sci & Res 2019, 10(1), 195-202.

A reliable, rapid, simple and accurate high-performance liquid chromatography method with UV detection was developed for the simultaneous quantitative determination of strychnine in a polyherbal formulation prepared from Nux Vomica. Krimimudgara rasa, a herbal dosage form containing Strychnos nux vomica, Apium graveolens, Embellia ribes, Butea monosperma in combination. Separation of the strychnine from its major and minor degradation products was successfully achieved on a reversed-phase C-18 column using (250 mm × 4.6 mm ID, 5 µm particle size), with isocratic elution using a mixture of Methanol: KH₂PO₄ buffer solution (10 mmol, adjusted to pH 3 with orthophosphoric acid) (50:50 v/v) at flow rate 0.7 ml/min at 254 nm. The method was validated concerning linearity, precision, accuracy, system suitability and robustness. The responses were linear in the drug concentration range of 1 - 10 μg/ml. The percent recoveries were in the range between 98 - 101 % from a mixture of degradation products. The utility of the procedure was verified by its application to a marketed formulation that was subjected to accelerated degradation studies. The method could distinctly separate the drug and degradation products. The products formed in marketed tablet dosage form were similar to those formed during stress studies.

8 illus, 6 tables, 25 ref

000159   ADHIHETTY N S, PADUMADASA C (Chemistry Dep, Sri Jayewardenepura Univ, Nugegoda 10250, Sri Lanka, Email: chayanika@sjp.ac.lk) : Correlation of variation in the percentage of compounds responsible for mosquito repellent activity in citronella oil over time with mosquito repellent efficacy of commercial citronella oil samples and sprays. Int J Pharm Sci & Res 2019, 10(1), 189-94.

The control of mosquitoes, which transmit deadly diseases, has become a significant public health concern globally. Protection against mosquito bites is an important part of preventing mosquito-borne diseases. Citronella oil extracted from two types of citronella grass Cymbopogon winterianus Jowitt (Java type) and Cymbopogon nardus (L.) Rendle (Ceylon type) possess compounds responsible for mosquito repellent activity. In the Sri Lankan market, there are some mosquito repellent products manufactured using citronella oil. In the present study, commercial citronella oil samples were subjected to GC-MS analyses weekly for sixteen weeks to investigate the variation in the percentage of compounds responsible for mosquito repellent activity with time and to correlate this variation to mosquito repellent efficacy of commercial citronella oil samples and sprays. In the tested samples, the percentages of compounds responsible for mosquito repellent activity as well as their mosquito repellent activity have shown a decline with time. The time duration that the maximum mosquito repellent activity would persist in the tested samples may be considerably lower than the shelf life stipulated. Therefore, one must consider this when relying on this mosquito repelling agents to prevent being bitten by mosquitoes.

7 illus, 11 ref

000303   SARAVANAN P C, KRISHNAN M M, ARUMUGHAM M N (Chemistry Dep, Thiruvalluvar Univ, Vellore - 632 115, Email: aru_mugham@yahoo.com) : DNA binding and cytotoxicity studies of ternary copper(II) complexes containing heterocyclic bases and thiourea. Int J Pharm Sci & Res 2019, 10(1), 148-56.

This article describes the Cu(II) complexes including [Cu(phen)(L-val)TU)] 1 & [Cu(bpy)(L-val)TU)] 2 (phen = 1, 10-phenanthroline; bpy = 2,2’-bipyridyl, L-val = L-valine and TU = Thiourea). The complexes were synthesized by ligand substitution method and characterized by various physicochemical techniques. The intense UV band around 270 nm was due to n-π* transition. The binding behaviors of these complexes to cal thymus DNA (CT-DNA) were explored by spectroscopic titrations, emissions, viscosity measurements, and cyclic voltammetry. The binding constant value of complexes 1 and 2 was 8.42 × 10⁵ M^-1 and 7.12 × 10⁵ M^-1 respectively. Results suggest that the complex 1 can bind to CT-DNA through intercalation and complex 2 binds through partial intercalation. However, their binding ability differed, this may be attributed to the difference in ligand coordinated the metal centre, complex 1 shows higher binding affinity than complex 2, this is due to the extended π-conjugated system of phenanthroline ring. The cytotoxicity of complexes 1 and 2 evaluated by MTT assay; results indicated that complexes have significant cytotoxicity with HePG2 tumor cell line.

8 illus, 3 tables, 31 ref

000276   PANDEY D, GUPTA A K (Bastar Vishwavidyalaya, Jagdalpur - 494 001, Email: pandey.dhananjay333@gmail.com) : Bioactive compound in Curcuma caesia (Roxb.) from Bastar and its spectral analysis by HPLC, UV-visible, FT-IR, NMR, and ESI-MS. Int J Pharm Sci & Res 2019, 10(1), 139-47.

The increasing failures of chemotherapeutics and antibiotic resistance exhibited by pathogenic microbes have led to the screening of several medicinal plants for their potential antimicrobial activity. Thus, the present endeavour deals with the exploration of antibacterial efficacy of Curcuma caesia (Roxb.) (Family Zingiberaceae) against bacterial cultures procured from IMTECH, Chandigarh as a screen for potential candidates for the development of natural antibiotics. The agar well diffusion assay was performed to screen antibacterial activity, and ZOI was recorded. The results were analyzed using one way ANOVA with DMRT. A broth macro-dilution assay was used to determine (MIC) and (MBC). Finally, the purified fraction was chemically characterized by spectral analysis. The antibacterial activity profile revealed that the methanolic root extract exhibited broad-spectrum antibacterial potentiality. The extract exhibiting the highest antibacterial activity was purified by column chromatography and further with HPLC, and TLC analyzed the band pattern. The bio-efficacy of the purified fraction was assessed against pathogenic bacteria, and the MIC and MBC were determined. The maximum zone of inhibition was recorded against B. cereus (MTCC 430) and K. pneumoniae (MTCC 3384). The purified fraction from a crude extract of C. caesia (Roxb.) indicates that the molecular weight of the purified compound is 368, the molecular formula is C₂₁H₂₀O₆. Its chemical characteristics and structural properties were found to be similar to that of 1, 7-bis (4-hydroxy-3-methoxyphenyl)-1,6-heptadiene-3,5-dione. However, this is the first report of the presence of curcumin in C. caesia (Roxb.) from Bastar demonstrating antibacterial property.

11 illus, 2 tables, 35 ref

000203   ESWARAMMA P, MURTHY K V R (Pharmaceutics Dep, Vagdevi Coll of Pharmacy, Gurazala - 522 415, Email: eswarivenni@gmail.com) : Evaluation of Moi gum in the formulation of controlled release matrix tablets using losartan potassium. Int J Pharm Sci & Res 2019, 10(1), 121-29.

Matrix tablets were developed using moi gum for investigating its suitability for the controlled release using losartan potassium as a model drug. Tablets were prepared by direct compression method. Lactose and dibasic calcium phosphate (DCP) were used as channelling agents. In-vitro studies were performed in 0.1N hydrochloric acid for the first two hours and pH 6.8 phosphate buffer for the next ten hours. The retardation of drug release was influenced by gum concentration and nature of diluents. The drug release was retarded when compared with dissolution patterns of synthetic polymers like polyethylene glycol (PEG 4000 & PEG 6000). The release rate, extent, and mechanisms were found to be governed by the concentration of the gum and channelling agents. Increased rate and extent of the drug release were found by using a higher content of channelling agent in the matrix due to increased porosity. It was found that type and concentration of channelling agent significantly affect the percentage drug release, release rate constant (K) and diffusion exponent (n). The FTIR studies confirmed that there was no interaction between the drug and moi gum.

5 illus, 12 tables, 19 ref

000285   PURI S K, HABBU P V, KULKARNI P V, KULKARNI V H (Pharmacognosy and Phytochemistry Dep, SET’s Coll of Pharmacy, Dharwad - 580 002, Email: smitamadagundi@gmail.com) : Hepatoprotective activity of fungal endophytic fractions of Andrographis paniculata (Burm. f.) Wall Nees. leaves in paracetamol and ethanol induced hepatotoxicity. Int J Pharm Sci & Res 2019, 10(1), 97-107.

The most widely used drug for analgesic and antipyretic is Paracetamol, but a change in dose at high-level yields to adverse reactions such as the toxic liver. The psychoactive compound present in alcoholic drinks is ethanol. Chronic alcohol consumption and various pathological conditions vary from basic intoxication to life-threatening pathological states. Endophytes are the microorganisms present inside the plant tissues forming a mutualistic, symbiotic and trophobiotic relationship. Endophytic organisms such as fungi, bacteria, and actinomycetes are found in all types of vascular plants and grasses. The present study reveals the protective effects of previously isolated fractions of A2EA (ethyl acetate) and A2nB (n-butanol), from the endophyte Preussia sp. PPV3.6 (APLF-2) isolated from Andrographis paniculata leaves on Paracetamol and ethanol-induced hepatotoxicity at a dose of (50 mg/kg & 100 mg/kg). A2EA and A2nB (50 mg/kg & 100 mg/kg) reversed the increased serum biochemical parameters such as serum glutamate oxaloacetate transaminase (SGOT), serum glutamate pyruvate transaminase (SGPT), serum alkaline phosphate (SALP), total bilirubin, direct bilirubin, total cholesterol (TC) and triglycerides(TG) as compared to Paracetamol and ethanol induced treated group (***p < 0.001). A2EA and A2nB (50 mg/kg & 100 mg/kg) significantly increased the total protein levels. A2EA and A2nB (100 mg/kg p.o) also restored the lipid peroxidation (LPO), superoxide (SOD) and catalase (CAT) levels.

4 illus, 4 tables, 33 ref

000184   BHORE P B, KHANVILKAR V V (Quality Assurance Dep, Bharati Vidyapeeth’s Coll of Pharmacy, Navi Mumbai - 400 614, Email: pranalibhore1994@gmail.com) : Silica gel: A keystone in chromatographic techniques. Int J Pharm Sci & Res 2019, 10(1), 12-22.

In research, the analyst gets samples for separation ranging from a simple mixture of two or more synthetic drugs to complex ones obtained from biological, environmental or industrial processes. Chromatography has extensively used in such separations where component separation based upon their affinity towards stationary phase and mobile phase. 90 % of the stationary phases available use silica gel either in its original form or with advanced surface properties. To furnish the reader with detailed information on silica gel, the functional moiety in chromatography, from its synthesis, properties, types, modification of surface characteristics and applications. We aim to focus on novel silica materials evolved recently and getting attention due to their performance.

9 illus, 5 tables, 13 ref

000261   MUKHERJEE S, GHOSH D, DE R K (Indian Statistical Institute, Kolkata - 700 108, Email: rajat@isical.ac.in) : Expected return time to the initial state for biochemical systems with linear cyclic chains: Unidirectional and bidirectional reactions. Sadhana 2019, 44(1), 3.

Biochemical systems are robust in nature. We define robustness of a biochemical system as the property where during time evolution, a closed system returns to its initial state. In this study, we propose some mathematical formulations to analyse the robustness of a closed biochemical system. We have provided a tentative guideline towards applying the theory to a non-closed system. We know that a biochemical system evolves with time as a continuous-time Markov process. When this Markov chain is irreducible, it can be proved theoretically that the system will always return to its initial state, and also the expected time of return can be determined. This return time depends upon the stationary probability distribution, which is determined as the solution of an eigenvalue equation xQ = 0 where Q is the transition rate matrix. We calculate this expected return time for five different closed systems: unidirectional cyclic linear chains, bidirectional cyclic linear chains and three real biological systems, and verify the theoretical results against the average return time obtained by stochastic simulation.

9 illus, 21 ref

000260   MISHRA L, SUNDARARAJAN M (Bhabha Atomic Research Centre, Mumbai - 400 085, Email: smahesh@barc.gov.in) : Quantum chemical studies of structures and spin Hamiltonian parameters of iron transferrin using isolated and embedded clusters models. J Chem Sci 2019, 131(2), 15.

Density functional theory (DFT) based calculations using large cluster models are used to elucidate the ground state electronic structure of iron bound transferrin. Explicit incorporation of second coordination amino acid residues and crystallographic water molecules anchors the active site. Our calculations clearly suggest that tyrosine amino acid (Tyr188) residue is bound to iron when the structures are optimized within the continuum solvation model. However, in the gas phase optimized structure, we note that Tyr188 is unbound to Fe (by more than 3 Å). The Mössbauer isomer shift (δ) and quadrupolar splitting ($∆$E_q) of iron transferrin are in line with the experimental data only when Tyr188 is bound to Fe(III). Further, the computed oxygen hyperfine coupling constant value is very large (−14.5 MHz) when bound to iron which can be verified through ¹⁷O NMR experiments. We propose that Tyr188 is strongly bound to Fe(III) at physiological pH, which needs to be protonated (acidic pH) to weaken this bond, thus the metal release pathway can be possible only in acidic conditions.

2 illus, 2 tables, 62 ref

000196   DAVE P, AGRAWAL B, THAKARDA J, BHOWMIK S, MAITY P (Gujarat Forensic Sciences Univ, Gujarat - 382 007, Email: pmaity@gfsu.edu.in) : An organometallic ruthenium nanocluster with conjugated aromatic ligand skeleton for explosive sensing. J Chem Sci 2019, 131(2), 14.

9-Ethynylphenanthrene (EPT) bound to highly monodispersed Ruthenium (Ru) nanocluster (Ru:EPT) with mean diameter of 1.5 ± 0.2 nm and mol wt. of $~$8600 Da was synthesized via a facile and high yield biphasic ligand exchange protocol using similar sized ethylene glycol (EG)-stabilized Ru clusters (Ru:EG) as precursor. The synthesized organometallic nanocluster was meticulously analyzed to understand its size distribution, oxidation state, crystallinity, optical and luminescence behavior and metal–ligand interfacial structure. Contrary to the extensive quenching of ligand emission by metalcore as usually observed, the ruthenium core here acts as a conductor, which conjugates surface ligands with strong emission property courtesy to an unusual vinylidene-binding motif. Thus, the synthesized nanocluster shows good luminescence property (φ = $~$ 7 %) originated from the ligand skeleton and the spherical metal core restricts lateral overlap of phenanthrene moiety to cause any excimer emission. This nanocluster showed high sensitivity for solution phase detection of nitroaromatic explosives through luminescence quenching method (K_SV up to 4.98 × 10⁴ M⁻¹) and mimic the mechanism like conjugated organic polymer. We propose that dynamic π − π interaction between Ru bound phenanthrene moiety and nitroaromatic compounds followed by photoinduced electron transfer (PET), as well as Förster Resonance Energy Transfer (FRET), are the possible mechanisms behind this luminescence quenching.

4 illus, 32 ref

000346   VINODKUMAR T, SUBRAMANYAM P, KUMAR K V A, REDDY B M, SUBRAHMANYAM C (Chemistry Dep, Indian Institute of Technology, Hyderabad - 502 285, Email: csubbu@iith.ac.in) : Construction of metal oxide decorated g-C₃N₄ materials with enhanced photocatalytic performance under visible light irradiation. J Chem Sci 2019, 131(2), 13.

Herein we report the synthesis and photocatalytic evaluation of heterostructure WO₃/g-C₃N₄ (WMCN) and CeO₂/g-C₃N₄ (CMCN) materials for RhB degradation and photoelectrochemical studies. These materials were synthesized by varying the dosages of WO₃ and CeO₂ on g-C₃N₄ individually and were characterized with state-of-the-art techniques like XRD, BET surface area, FT-IR, UV–Vis DRS, TGA, SEM, TEM and XPS. A collection of combined structural and morphological studies manifested the formation of bare g-C₃N₄, WO₃, CeO₂, WO₃/g-C₃N₄ and CeO₂/g-C₃N₄ materials. From the degradation results, we found that the material with 10 wt % WO₃ and 15 wt % CeO₂ content on g-C₃N₄ showed the highest visible light activity. The first order rate constant for the photodegradation performance of WMCN10 and CMCN15 is found to be 5.5 and 2.5 times, respectively, greater than that of g-C₃N₄. Photoelectrochemical studies were also carried out on the above materials. Interestingly, the photocurrent density of WMCN10 photoanode achieved 1.45 mA cm⁻² at 1.23 V (vs.) RHE and this is much larger than all the prepared materials. This enhanced photoactivity of WMCN10 is mainly due to the cooperative synergy of WO₃ with g-C₃N₄, which enhanced the visible light absorption and suppresses the electron–hole recombination.

8 illus, 1 table, 42 ref

000161   AKREMI A, NOUBIGH A (Chemistry Dep, Northern Border Univ, Arar 91431, Kingdom of Saudi Arabia, Email: akrimimi@gmail.com) : New organotin(IV) chlorides derived from N-(2-hydroxyphenyl)aryloxy sulfamates: Synthesis, characterization and DSC investigation. J Chem Sci 2019, 131(2), 12.

Three monomeric pentacoordinate organotin complexes were prepared by the reaction of dimethyltin dichloride with three N-(2-hydroxy)phenyl substituted aryloxy sulfamates in alkaline medium. The newly synthesized compounds were characterized on the basis of their infrared, CPMAS NMR, powder XRD diffraction and elemental analysis. The XRD powder analyses revealed a tetragonal system for two complexes, whereas the third one was crystallized in the hexagonal system. The thermal decomposition behavior of the synthesized complexes have been investigated and all the organotin compounds have a similar order of thermal stability.

4 illus, 3 tables, 44 ref

000207   FEMINUS J J, MANIKANDAN R, NARAYANAN S S, DEEPA P N (Analytical Chemistry Dep, Madras Univ, Chennai - 600 025, Email: pndeepa@hotmail.com) : Determination of gallic acid using poly(glutamic acid): Graphene modified electrode. J Chem Sci 2019, 131(2), 11.

Gallic acid (GA) is one of the main phenolic components occurring naturally in plants and has been a subject of increasing interest owing to its antioxidant, anti-mutagenic and anti-carcinogenic properties. The present work describes a rapid and cost-effective analytical procedure for the determination of gallic acid. PolyGlu/rGO electrode was fabricated by the electro-polymerisation of glutamic acid on reduced graphene oxide (rGO) modified paraffin impregnated graphite electrode (PIGE). The modified electrode was characterized by SEM, AFM and ATR-IR. The electrochemical behavior of gallic acid at the modified sensor was studied by voltammetric and amperometric techniques under optimized conditions in pH 5 acetate buffer. The electrode showed good linear response towards the determination of gallic acid over the range of 0.03–480 µM with 0.01 µM as the detection limit for voltammetric technique and the amperometric technique showed a linear range of 1–17 µM with 0.33 µM as the detection limit. The electrode also showed good stability and reproducibility with a sensitivity of 0.97 µM/µA. The proposed method can be applied to detect GA in real samples with satisfactory results.

11 illus, 2 tables, 49 ref

000352   YUN D, CHAE J B, KIM C (Fine Chemistry Dep, Seoul National Univ of Science and Technology, Seoul 129-743, Republic of Korea, Email: chealkim@seoultech.ac.kr) : A novel benzophenone-based colorimetric chemosensor for detecting Cu²⁺ and F⁻. J Chem Sci 2019, 131(2), 10.

A novel selective colorimetric chemosensor ANBP ((E)-(2-(((8-hydroxy-2,3,6,7-tetrahydro-1H,5Hpyrido[3,2,1-ij]quinolin-9-yl)methylene)amino)-5-nitrophenyl)(phenyl)methanone), based on the combination of benzophenone group and julolidine chromophore, was synthesized. Sensor ANBP showed rapid colorimetric responses toward Cu²⁺ (pale orange to pink) and F⁻ (orange to blue). The detection limit by ANBP to Cu²⁺ (6.82 µM) was far below WHO guideline value (31.3 µM). Moreover, ANBP could quantify Cu²⁺ in aqueous samples. 1:1 binding mode between ANBP and Cu²⁺ or F⁻ was proposed by ESI-mass analyses and Job plots. The remarkable color changes with Cu²⁺ and F⁻ resulted from the intramolecular charge transfer (ICT) effect, which was demonstrated by theoretical calculations.

7 illus, 1 table, 55 ref

000191   CHANU S B, RAZA M K, BANERJEE S, MINA P R, MUSIB D, ROY M (Chemistry Dep, National Institute of Technology, Manipur - 795 004, Email: mithunroy@nitmanipur.ac.in) : ROS dependent antitumour activity of photo-activated iron(III) complexes of amino acids. J Chem Sci 2019, 131(2), 9.

Several amino acid-based photo-active monomeric iron(III) complexes of the general formula, [Fe(L)₂]⁻, where L = Schiff base ligands (salisalidene arginine, salicylidenetryptophan, 3,5-di-tert-butyl benzalidine arginine and salicylidene tryptophan) were synthesized, characterized and explored for photoactivated anticancer activity to Chang Liver Cells, HeLa and MCF-7 cells. Complexes exhibited remarkable photo-cytotoxicity with IC₅₀ value to the extent of 0.7 μM to Chang Liver Cells in visible light and there was a 40-fold enhancement in cytotoxicity in comparison to the cytotoxicity in dark. Complexes were non-toxic to MCF-10A (normal cells) in dark and visible light (IC₅₀ > 100 μM in dark; IC₅₀ > 80 μM in visible light) signifying target-specific nature of the anti-tumour activity of the complexes. Increased ROS concentration, as probed by DCFDA assay, in the cancer cells was responsible for apoptotic cell death. Decarboxylation or phenolate-Fe(III) charge transfer of photo-activated iron(III) complexes generating •OH radicals (ROS) were responsible for the apoptosis. Overall, the tumour-selective photo-activated anticancer activity of the amino acidbased iron(III) complexes have shown a promising aspect in developing iron-based photo-chemotherapeutics as the next generation PDT agents.

6 illus, 1 table, 37 ref

000349   YALAVARTHI N R, GUNDOJU N, BOKAM R, PONNAPALLI M G (CSIR-Indian Institute of Chemical Technology, Telangana - 500 007, Email: mangala@iict.res.in) : Cu-doped zeolitic imidazolate framework catalysed highly selective conversion of alkynes to β-keto and vinyl sulfones using sodium sulfinates. J Chem Sci 2019, 131(1), 8.

Cu²⁺-doped zeolitic imidazolate framework-8 (ZIF-8)-catalyzed one-pot procedure to synthesize β-keto and vinyl sulfones by the direct oxysulfonylation and hydrosulfonylation of alkynes via radical reaction under mild conditions has been described. The advantages of this protocol included broad substrate scope and excellent β-keto and E-stereoselectivity. The Cu/ZIF-8 catalyst not only exhibited excellent performance but also had a great stability in the reaction, successfully allowing its reuse up to five cycles. This efficient Cu/ZIF-8 heterogeneous catalyst is explored for the first time to generate β-keto and vinyl sulfones.

4 tables, 42 ref

000227   JOSHI A, VAIDYA S, SINGH M (Institute of Nano Science and Technology, Punjab - 160 062, Email: monika@inst.ac.in) : Synthesis and structure of Anderson cluster based organic–inorganic hybrid solid, [{Cu(2- pzc)(H₂O)₂}₂ {H₇AlMo₆O₂₄}] · 17H₂O and its dye adsorption properties. J Chem Sci 2019, 131(1), 7.

An inorganic–organic hybrid compound, namely [{Cu(2-pzc)(H₂O)₂}₂{H₇AlMo₆O₂₄}]·17H₂O was synthesized based on Anderson–Evans cluster by the normal stirring process at room temperature. Its structure consists of metal coordination polymer covalently linked with Anderson–Evans cluster forming a 2D-sheet with void space containing water chains as determined by Single-Crystal X-ray Diffraction technique. This material owing to its void space of approx. 13 Å was utilized for adsorption of organic dyes like Methylene Blue (MB), Basic Violet 1 (BV1) and shows ultra-high uptake (more than 90 %) within 5 min.

12 illus, 1 table, 36 ref

000198   DEVI S P, LYNGDOH R H D (Chemistry Dep, North-Eastern Hill Univ, Meghalaya - 793 022, Email: rhdl@nehu.ac.in) : Uncatalyzed gas phase aziridination of alkenes by organic azides. part 2. Whole azide reaction with alkene. J Chem Sci 2019, 131(1), 6.

The B3LYP/6-31G(d,p) DFT method was used to study alkene aziridination by azides through uncatalyzed thermal gas phase routes which involve the whole azide reactant molecule without dissociation. Two mechanisms were studied – Route I involving concerted azide addition to alkene with the elimination of N₂, and the multi-step Route II involving 1,3-dipolar cycloaddition between azide and alkene. Three azides RN₃ (R = H, Me, Ac) are reacted with alkene substrates forming aziridine products. The concerted addition– elimination step of Route I is exothermic with an appreciable barrier, where the facility order Ac > Me > H points to electrophilicity of the azide reactant. The initial 1,3-dipolar cycloaddition step of Route II involves smaller barriers than Route I, while thermal decomposition of the triazoline intermediate to aziridine and N₂ involves two more steps with an N-alkylimine intermediate. The very high barrier for N-alkylimine cyclization to aziridine could be offset by the high exothermicity of the previous step. Geometries of the transition states for various reaction steps studied here are described as ‘early’ or ‘late’ in good accordance with the Hammond postulate. Two other mechanisms (Routes A and B) studied earlier (involving discrete nitrene intermediates) are compared with Routes I and II, where Route II involving 1,3-dipolar cycloaddition is predicted to be energetically the most favored of all the four mechanisms for thermal gas-phase aziridination of alkenes by azides.

7 illus, 4 tables, 40 ref

000304   SASIKUMAR D, KOHARA R, TAKANO Y, YUYAMA K-I, BIJU V (Hokkaido Univ, Sapporo 001-0020, Japan, Email: tak@es.hokudai.ac.jp) : Kinetics of singlet oxygen sensing using 9-substituted anthracene derivatives. J Chem Sci 2019, 131(1), 5.

Singlet oxygen (¹O₂), the lowest excited-state of molecular oxygen receives great attention in basic research and clinical and industrial settings. Despite several spectroscopic methods available for ¹O₂ sensing, fluorescence sensing receives great attention, for which many fluorogenic sensors based on substituted anthracene are reported. Nonetheless, the roles of substituents on the sensing efficiency, in terms of detection time, remain largely unknown. In this work, we examine the ¹O₂ sensing efficiency of a fluorescence sensor based on a coumarin–anthracene conjugate, which is an electron donor-acceptor dyad, and compare the efficiency with that of 9-methylanthracene. Here, ¹O₂ is generated using the standard photosensitizer Rose Bengal, which is followed by estimation of the rate of reaction of ¹O₂ to the sensor and 9-methylanthracene. The second order reaction rate of the sensor is an order of magnitude less than that of 9-methylanthracene. The lower reactivity of the sensor to ¹O₂ suggests that the roles of substituents, such as electronic interactions, steric interactions and the reactivity of precursor complexes, on sensing efficiency should be carefully considered during construction of fluorogenic molecular sensors.

4 illus, 34 ref

000287   RAHMAN T, BORAH G, GOGOI P K (Chemistry Dep, Dibrugarh Univ, Assam - 786 004, Email: geetikachem@yahoo.co.in) : Hybrid composite of CuO with g-C₃N₄ as a photoactive catalyst: An efficient approach for the oxidation of alcohols. J Chem Sci 2019, 131(1), 4.

An eco-friendly method for the oxidative transformation of alcohols to their corresponding carbonyl compounds by using g-C₃N₄@CuO as a photoactive heterogeneous catalyst has been developed. The catalyst was characterized by SEM-EDX, TEM, BET surface area measurements, powder XRD, FTIR, photoluminescence and UV-Vis spectroscopy. It was found to be very effective for the conversion of both primary and secondary alcohols into aldehydes and ketones with excellent yields using tert-butyl hydrogen peroxide (TBHP) as oxidant at room temperature in the presence of visible light in aqueous medium. The catalyst can be separated from the reaction mixture by simple centrifugation and reused up to five cycles without significant loss in activity.

5 illus, 5 tables, 43 ref

000239   KONER A, SATHYAMURTHY N (Jawaharlal Nehru Centre for Advanced Scientific Research, Karnataka - 560 064, Email: nsathyamurthy@gmail.com) : Stabilizing influence of silicon substitution on dibenzene and its isomers. J Chem Sci 2019, 131(1), 3.

The stabilizing effect of silicon substitution on sixteen different isomers of dibenzene (C₁₂H₁₂) has been investigated using second-order Møller-Plesset perturbation (MP2) theory and the cc-pVDZ basis set. While the most stable isomers of Si₁₂H₁₂ have only Si–Si bonds, some of the stable isomers have isolated Si=Si bonds and may be amenable to experimental observation. Vibrational frequencies were calculated for the optimized geometries at the Hartree-Fock level of theory to ensure that they corresponded to true minima on the potential energy landscape. Natural bonding orbital analysis confirms the existence of isolated Si=Si double bonds in some of the isomers. Dipole moment values were determined to check for the presence of centre of symmetry in certain geometries.

5 illus, 1 table, 12 ref

000267   NAWAB M, BAROT S, BANDYOPADHYAY R (Science Dep, Pandit Deendayal Petroleum Univ, Gujarat - 382 007, Email: rajib.bandyopadhyay@sot.pdpu.ac.in) : Nano-sized Silicalite-1: Novel route of synthesis, metal impregnation and its application in selective oxidation of toluene. J Chem Sci 2019, 131(1), 2.

The novel route of synthesis and catalytic performance of nano-sized Silicalite-1 are presented. Nano-sized Silicalite-1 was initially obtained from a clear solution using sodium silicate as silica source and tetrapropylamonium hydroxide as a template. The effects of silica source on the product yield, purity, crystallization rate and crystallinity were investigated. Effect of seeds in the synthesis was also studied. Nucleation time decreased to 6 h from 24 h using 4 % seed, with yield and crystallinity 70 % and 90 %, respectively. The catalyst was characterized by XRD, FE-SEM, TG, FITR and N₂ adsorption–desorption techniques. Transition metals like Fe, Cu and Mo were impregnated by wet impregnation method. Cu-impregnated nanosized Silicalite-1 was found to be highly active for the oxidation of toluene with H₂O₂.

9 illus, 3 tables, 44 ref

000199   DEY G R (Radiation and Photochemistry Div, Homi Bhabha National Institute, Maharashtra - 400 085, Email: grdey@barc.gov.in) : Effect of phenyl moiety on the formation of radicals and radical cations of thioamides in n-butyl chloride: A pulse radiolysis study. J Chem Sci 2019, 131(1), 1.

The formation of radical cations and radicals of thioamides (R)(NH₂)CS, where R represents CH₃ in thioacetamide (TA) and C₆H₅ in thiobenzamide (TBA) in n-butyl chloride has been studied using pulse radiolysis technique. The radical cations of TA and TBA are observed in n-butyl chloride, and on their subsequent deprotonation, respective radicals are generated. In this study on thioamide solutions in n-butyl chloride, the transient species formed at 1.2 μs after the electron pulse exhibiting absorption maxima in 400 nm region are attributed to their radical cations. In the presence of 0.1 M ethanol (C₂H₅OH), a radical cation scavenger, the absorbance values at corresponding peaks are reduced substantially, revealing the formation of their respective radical cations. Moreover, at a later time, the generation of radical species takes place through deprotonation of radical cations and also through direct reactions during electron pulse irradiation. The mechanisms for the formation of radical cations and radicals of these two thioamides under pulse radiolysis have been revisited in butyl chloride medium wherein the charge transfer reactions are more prominent. Results of quantum chemical calculation support the mechanistic explanation and provide information on the reactivity of parent molecules, and the charge distribution on radical cations and radicals species of thioamides.

4 illus, 1 table, 14 ref

000172   ASAI K, OCHIAI A, KAWASHIMA N, TOKUOKA Y (Toin Univ of Yokohama, Yokohama 225-8503, Japan, Email: tokuoka@toin.ac.jp) : Effect of ethanol on iontophoretic transdermal delivery of 5-aminolevulinic acid through Yucatan micropig full-thickness skin. Indian J Pharm Sci 2019, 81(1), 177-81.

The effect of ethanol was investigated on iontophoretic transdermal delivery of 5-aminolevulinic acid through Yucatan micropig full-thickness skin. When 20 % ethanol was added into an aqueous 5-aminolevulinic acid solution, the iontophoretic permeation of 5-aminolevulinic acid through Yucatan micropig full-thickness skin was enhanced. The addition of ethanol also enlarged the partition of 5-aminolevulinic acid into Yucatan micropig full-thickness skin, which gave rise to enhancement of 5-aminolevulinic acid permeation. This result suggested that the combination system of iontophoretic delivery and 20 % ethanol could be a promising approach for the promotion of 5-aminolevulinic acid skin permeation.

2 illus, 1 table, 30 ref

000210   GIRISH K, CHANNU B C, BABA A R (Chemistry Dep, Maharani’s Science Coll for Women, Mysuru - 570 005, Email: arbaba71@rediffmail.com) : Synthesis and antibacterial activity of cobalt(II) complex of curcumin. Indian J Pharm Sci 2019, 81(1), 150-5.

To improve the bioavailability of curcumin numerous approaches were attempted, which included complexation with metal ions. In the present study, a metal ion complex of cobalt(II) with curcumin was synthesized and screened for in vitro antibacterial activity in comparison with curcumin on seven bacterial strains, Bacillus subtilis, Escherichia coli, Klebsiella pneumoniae, Salmonella typhi, Shigella flexneri, Proteus vulgaris and Staphylococcus aureus. The cobalt-curcumin complex was effective against all strains tested and the activity was greater than that exhibited by curcumin. Comparison of the inhibitory activity with the macrolide antibiotic azithromycin revealed that cobalt-curcumin complex was as active as the antibiotic. The cobalt-curcumin complex could be a suitable candidate for further in vivo investigations. This is the first report of antibacterial activity of cobalt-curcumin complex against all the bacterial strains tested except Escherichia coli.

3 illus, 2 tables, 31 ref

000301   SANAROVA E, LANTSOVA A, OBOROTOVA N, POLOZKOVA A, DMITRIEVA M, ORLOVA O, NIKOLAEVA L, BORISOVA L, SHPRAKH Z (Research Institute of Experimental Diagnostics and Therapy of Tumors, Moscow- 115 478, Russia, Email: sanarova8686@mail.ru) : Development of a liposomal dosage form for a new somatostatin analogue. Indian J Pharm Sci 2019, 81(1), 146-9.

A new pentapeptide analogue of somatostatin was synthesized and preliminary studies demonstrated that this analogue possessed antitumor activity on transplanted solid tumours of mice. Due the analogue’s insolubility in water, a liposomal formulation was attempted to increase bioavailability of the drug, to administer intravenously and to improve selectivity towards the tumor cells. This study employed the somatostatin analogue, egg lecithin, 1,2-distearoyl-sn-glycero-3-phosphoethanolamine-N-[methoxy (polyethyleneglycol)-2000, cholesterol and sucrose. Model compositions of the somatostatin analogue liposomal dosage form were prepared using the lipid film rehydration method. All samples obtained were characterized by measuring size of liposomes, pH of the liposomal dispersion, and assay of somatostatin analogue incorporated in the liposomal bilayer. Efficiency of the formulation was investigated on models of breast adenocarcinoma Ca-755. During experimental development of the somatostatin analogue liposomal formulation, an optimal composition was established, which included egg lecithin and 1,2-distearoyl-snglycero-3-phosphoethanolamine-N-[methoxy(polyethyleneglycol)-2000 in the 72/1 molar ratio. Influence of extrusion on the quality of liposomal preparations was studied. It was shown that to reach an optimal liposome size of about 150 nm, 7 extrusion cycles were necessary. In addition, while assessing the stability of the somatostatin analogue liposomal dispersion during storage it was found that somatostatin analogue was extremely unstable in liquid form, thus, to produce a stable formulation, lyophilization became necessary. The liposomal formulation when tested on transplanted tumours in mice, more than 60 % tumor growth inhibition was observed at 5 mg/kg dose and more than 80 % tumor growth inhibition at 20 mg/kg dose. These findings indicated that further efforts are required to improve this liposomal formulation to develop the somatostatin analogue in to a potential antitumor drug.

2 illus, 3 tables, 8 ref

000351   YUAN G, ZHANG R, LI X, LI W, LI R, WANG B, GUO R (Qilu Hospital of Shandong Univ, Jinan, China, Email: grc7636@126.com) : Simultaneous HPLC-MS determination of loganin, morroniside and paeoniflorin in rat plasma; Pharmacokinetics of Liuwei Dihuang pills. Indian J Pharm Sci 2019, 81(1), 129-37.

A novel high performance liquid chromatography-mass spectrometry method for simultaneous determination of loganin, morroniside and paeoniflorin in rat plasma was developed, validated and applied to pharmacokinetic study of Liuwei Dihuang pills. Samples were prepared by liquid-liquid extraction with ethyl acetate. Separation was performed on a Wondasil C₁₈ column (150×4.6 mm, 5 μm) using a mixture of methanol and 0.02 % formic acid water solution (28:72, v/v) as the mobile phase. The flow rate and column temperature were set at 0.7 ml/min and 30°. The compounds were detected in selected ion monitoring mode using an ESI source in the negative mode. The method was linear over the ranges of 5-1000 ng/ml for the three analytes, with all determined correlation coefficients exceeding 0.993. All of the lower limits of quantification of the three analytes were 5 ng/ml. The intra-day and inter-day precisions were less than 7.50 %, and the accuracy ranged from –6.57 to 7.90 %. The mean recoveries of the analytes were higher than 68.86 %, and the matrix effects were between 92.35 and 103.54 %. This method was simple, sensitive and reliable, and could be used to monitor pharmacokinetics of loganin, morroniside and paeoniflorin. Moreover, this study might be helpful for quality control and guiding the clinical application of Liuwei Dihuang pills.

3 illus, 3 tables, 23 ref

000231   KAUR D, KAUR J, KAMAL S S (Rayat-Bahra Institute of Pharmacy, Hoshiarpur - 146 001, Email: jaspreet.meehnian@gmail.com) : Development and validation of a UV spectrophotometric method for determination of diacerein in bulk and a capsule dosage form. Indian J Pharm Sci 2019, 81(1), 124-8.

A simple, accurate and selective UV-spectrophotometric method was developed for the estimation of diacerein in bulk and pharmaceutical dosage forms. The method was developed and validated according to International Conference on Harmonization (ICH Q2 R1) guidelines. The developed method was validated statistically with respect to linearity, range, precision, accuracy, ruggedness, limit of detection and limit of quantitation. The study was carried out in citrate buffer pH 6.0 and λ_max was found to be 258.8 nm. Pure drug concentration was prepared in the range of 1-10 μg/ml and the linear regression analysis data showed good linear relationship with an R² value of 0.999. The limit of detection and limit of quantitation were found to be 0.675 and 1.189 μg/ml, respectively. Recoveries were found to be in the range of 100.815 to 101.744 % and % RSD was less than 2 %, which indicated that the developed method was accurate, precise, specific, rapid and suitable for the analysis of commercial samples.

3 illus, 5 tables, 24 ref

000176   BAHMANI Y, BAHRAMI T, ALIABADI A (Medicinal Chemistry Dep, Kermanshah Univ of Medical Sciences, Kermanshah, Iran, Email: aliabadi.alireza@gmail.com) : Synthesis, cytotoxicity assessment and molecular docking of n-(5-(substituted-benzylthio)-1,3,4- thiadiazole-2-yl)-2-p-fluorophenylacetamide derivatives as tyrosine kinase inhibitors. Indian J Pharm Sci 2019, 81(1), 63-70.

Compounds containing 1,3,4-thiadiazole nucleus appear to be potential tyrosine kinase inhibitors. Previous reports showed that some 1,3,4-thiadiazole derivatives were designed as probable tyrosine kinase inhibitors. Thiol derivative (2) was obtained from the reaction of 5-amino-1,3,4-thiadiazole-2-thiol with 4-fluorophenylacetic acid, ethyldimethyaminopropylcarbodiimide and hydroxybenzotriazole. Subsequent reaction of the obtained thiol derivative with diverse benzyl chlorides afforded the final compounds 3a-3l in a click reaction surprisingly. Derivatives with electron withdrawing moieties (F, Cl) exerted higher yield compared to methoxylated derivatives as electron donating group. Besides, docking studies using ArgusLab 4.0 was done for exploring the probable binding mode and interactions. Investigation of cytotoxicity of target compounds (3a-3l) by MTT assay revealed that these derivatives are more active against the breast cancer cell line MCF-7 and most of these were found to be more effective than imatinib as reference drug. Chlorine containing derivatives at ortho and meta positions were the most cytotoxic in these series.

3 illus, 2 tables, 27 ref

000187   CHAMLE A H, SHANE N L J, PAI A, MUDDUKRISHNA B S (Pharmaceutical Quality Assurance Dep, Manipal Coll of Pharmaceutical Sciences, Manipal - 576 104, Email: krishna.mbs@manipal.edu) : Photodegradation of methylcobalamin and its determination in a commercial formulation. Indian J Pharm Sci 2019, 81(1), 57-62.

Methylcobalamin is a highly photolabile and unstable molecule and hence, studies regarding photodegradation of methylcobalamin were carried out. In order to investigate the stability studies, the drug was subjected to photodegradation by exposing it to different light conditions in the validated photostability chamber as per ICH Q1B guideline. The drug was found to be less degraded in the blue light and was more prone to degradation under fluorescent light. Validated stability indicating liquid chromatography method was used for separating the methylcobalamin and its degradation products. The methylcobalamin peak with a retention time of 2.978 min was observed to decrease with a commensurate increase in a degradant peak at 4 min. The observed degradant peak was suspected to be hydroxocobalamin and was further confirmed by molecular weight determination. The fractions collected from high performance liquid chromatography were later injected into mass detector to determine the mass of the degradation products, which was found to be 665.78 amu.

7 illus, 4 tables, 11 ref

000344   VEERUBHOTLA K, WALKER R B (Pharmaceutics Div, Rhodes Univ, Grahamstown 6140, South Africa, Email: r.b.walker@ru.ac.za) : Development and validation of a stability-indicating RP-HPLC method using quality by design for estimating captopril. Indian J Pharm Sci 2019, 81(1), 45-56.

The applicability of a quality by design framework for the development of a sensitive, simple and selective, stability-indicating reversed-phase high-performance liquid chromatography analytical method for the analysis of captopril was investigated. Design of experiments using a central composite design approach was used for method development. Twenty experimental runs were performed with acetonitrile content ranging between 28 and 36 % v/v, pH from 2.8 to 3.6 and temperature between 22° and 32°. The experimental data obtained was used to derive a quadratic model for the retention time of captopril. The optimized method produced sharp peaks with good resolution (> 2) for captopril and the internal standard with retention times of 3.1 and 6.2 min, respectively. The experimental data revealed that acetonitrile content in the mobile phase and pH are significant factors that affect the retention time and resolution of captopril. Normal probability plots revealed that the residual and predicted data fall approximately on a straight line, indicating that the experimental error for these studies was evenly distributed suggesting that the model could be used to navigate the design space. This approach is useful to expedite method development and optimization activities in analytical laboratories.

5 illus, 6 tables, 35 ref

000318   SONI M (Chemistry Dep, D.A.V Coll, Abohar, Punjab) : Spectrophotometric determination of iron (III) in tap water using 8-hydoxyquinoline as a chromogenic reagent. J Pharmacogn Phytochem 2019, 8(1), 227-30.

A simple, rapid and sensitive spectrophotometric method was developed for the determinationation of trace amounts of iron (III) using 8-hydroxyquinoline as a chromogenic reagent. The proposed method was based on the reaction of iron (III) with 8-hydroxyquinoline in chloroform solution to form a metaloxine complex having a maximum absorption at 359 nm. Beers law was obeyed in the range of 1 to 14 ug/ml Fe3+. The recovery was between 98.60 and 103.30 % with a coefficient of variation of 1.209 %. The method was successfully applied to tap water samples and comparison with standard method showed the new method to be accurate and precise as the more sophisticated AAS commonly used for Fe determination.

2 illus, 3 tables, 8 ref