005165   GOYAL P K, BALTE A, AGGARWAL R R, SOLUNKE A, SAIKH F, BHAGWAT R (Chemistry Dep, Career Point Univ, Rajasthan- 324 001, Email: pgoyal_chem1981@yahoo.co.in) : Synthesis of some novel oxadiazole, thiadiazole and triazole derivatives of N-(2-methyl-5-aminophenyl)-4-(3- pyridyl)-2-pyrimidine amine as potential cytotoxic agents. J Chem Chem Sci 2019, 9(9), 239-48.

In this paper the synthesis of some novel 1,3,4-oxadiazoles, 1,3,4-thiadiazole and 1,2,4-triazoles derivatives of N-(2-methyl-5-aminophenyl)-4-(3-pyridyl)-2- pyrimidine amine have been carried out. N-(2-methyl-5-aminophenyl)-4-(3-pyridyl)- 2-pyrimidine amine was treated with methylchloroformate to give the corresponding methyl N-alkyl carbamate1, which converted to 4-alkyl semicarbazide2 by their reaction with hydrazine hydrate in ethanol. Compound 2 was treated with ammonium thiocyanate / hydrochloric acid to give substituted thiosemicarbazides3. The thiosemicarbazides were treated with concentrated sulfuric acid or sodium hydroxide solution to give 5-amino-2-methyl amino-1,3,4-thiadiazole 5 and 5-methyl amino1,2,4-triazoles-3-thiol 6 respectively. The substituted thiosemicarbazide was converted to 3,4-diamino-5-methyl amino-1,2,4-triazole 9 by its reaction with hydrazine hydrate. Compound 2 was treated with carbon disulfide in potassium hydroxide to give substituted oxadiazoles4. The reaction of 1,3,4-oxadiazoles with hydrazine hydrate gave substituted 1,2,4-triazoles 7, while compound 2 gave 4-amino-3,5-dicyclohexyl amino-1,2,4-triazole 8 upon heating at 90-120 °C. The structure of the synthesized compounds were confirmed by spectral and physical methods. All the synthesized compounds were evaluated for their in-vitro cytotoxicity against human lung carcinoma cell line A549 and Human colorectal adernocarcinoma cell line HT-29 by MTT assay method. Compound 7exhibited highest cytotoxicity against human lung carcinoma A549 cell line (IC50 06.5 μ g) and human colon carcinoma HT-29 cell line (IC50 06.0 μ g) among the derivatives.

3 tables, 26 ref

005170   KALHANS M B (Chemistry Dep, Bareilly Coll, Bareilly- 243 005, Email: drmbkalhans@gmail.com) : Study of softness indices and activity parameters in isomeric diazines by DFT method. J Chem Chem Sci 2019, 9(9), 234-8.

DFT method is more advance and gave better results than Hartree-Fock calculations. Quantum mechanical frame work of HSAB principle was given by Klopmann. The values of Em# for the two nitrogen’s were calculated, by applying DFT, which gave important results about the activity.

5 tables, 21 ref

005180   KUMAR S S, GHOSH S, SAHU M, GANESAN R (Homi Bhabha National Institute, Kalpakkam- 603 102, Email: rajesh@igcar.gov.in) : Molar heat capacity measurement of CaHCl and CaHBr. J Chem Sci 2019, 131(9), 100.

Molar heat capacities of two hydride ion conductors, namely, CaHCl and CaHBr, were measured by differential scanning calorimetry. The measured molar heat capacity data of these compounds as a function of temperature is given by the following expressions:

C_p < CaHCl > (J K^-1 mol^-1) = 57.806 + 16.420 x 10^-3 .T - 1.006 x 10⁶ .T^-2 (308–748 K)

C_p < CaHBr > (J K^-1 mol^-1 ) = 56.534 + 44.880 9 10^-3 .T - 1.481 x 106 .T^-2 (323–713 K)

From the above expressions, molar enthalpy increments, entropies and Gibbs energy functions of these compounds were derived and reported.

5 illus, 3 tables, 10 ref

005155   DAS T K, KUMAR A, RUZ P, BANERJEE S, SUDARSAN V (Homi Bhabha National Institute, Mumbai- 400 094, Email: vsudar@barc.gov.in) : Hydrogen storage properties of Ti₂FeV BCC solid solution. J Chem Sci 2019, 131(9), 98.

This paper deals with hydrogen storage properties of Ti-V based BCC solid solution incorporated with Fe. The alloy with composition Ti₂FeV was prepared by arc melting method. X-ray diffraction (XRD) and energy dispersive X-ray analysis studies confirmed formation of solid solution phase with uniform composition and BCC structure. SEM studies revealed the formation of irregular shaped particles with size in the range of few microns up on hydrogenation of the parent alloy. The alloy shows maximum hydrogen storage capacity of 3.41 wt. % at 20 bar and 303 K and the thermodynamic parameters established near room temperature suitability of the alloy for solid state hydrogen storage applications. Hydrogenation kinetics is found to be quite fast and detailed kinetic analysis were done to underscore the hydrogenation mechanism. Activation energy during the initial stage of hydrogenation is found to be 30.8 kJ/mol. The value decreases to 14.4 kJ/mol for extended duration of hydrogenation, and this is explained based on difference in rate determining steps existing at different time scales.

7 illus, 3 tables, 22 ref

005203   RAO P R V (Homi Bhabha National Institute, Mumbai- 400 094, Email: vasudeva@hbni.ac.in) : Materials for nuclear industry: Some historical perspectives. J Chem Sci 2019, 131(9), 97.

Materials play a key role in the safe and economical operation of nuclear reactors. Materials used in reactors also have to meet stringent chemical specifications for efficient performance. Commercial scale realization of nuclear materials has been a challenge to the nuclear industry. The history of development of nuclear materials has fascinating and unique examples of theoretical prowess as well as innovative experimentation and success in nuclear material development is characterized by synergy between the domains of laboratory research and industry. This paper describes the development of some of the important nuclear materials (uranium, plutonium, zirconium, boron, sodium and graphite), providing a historical perspective.

30 ref

005141   ACHARY S N, KATARI V, SAYED F N, TYAGI A K (Chemistry Div, Bhabha Atomic Research Centre, Mumbai- 400 085, Email: sachary@barc.gov.in) : A brief review on the effect of preparation conditions on magnetic properties of some A₂MMnO₆ (A = La, Eu and Y; M = Mg, Co, Ni) type perovskites. J Chem Sci 2019, 131(9), 96.

In this article, structural and magnetic properties of a number of A₂MMnO₆ (A = La, Eu and Y; M = Mg, Co, Ni) type perovskites prepared under different oxygen partial pressure are compared. The results indicated that both structure and magnetic properties of such materials are sensitive to preparation conditions, which in general is governed by the nature of transition metal ions as well as rare-earth ions. It was also pointed out that even though the deviation in structure is only marginal, they affect appreciably to their magnetic properties.

6 illus, 44 ref

005169   KAIM W (Stuttgart Univ, Stuttgart- 70550, Email: kaim@iac.uni-stuttgart.de) : Materials with electronic transitions in the near-infrared. J Chem Sci 2019, 131(9), 95.

Concepts have been developed which favor low-energy absorption in the near-infrared (NIR) region. These include metal-metal charge transfer (inter-valence charge transfer) transitions of mixed-valent species, radical ion compounds (anions, cations), and mixtures thereof. Recent examples from ruthenium coordination chemistry are presented in order to illustrate analysis and assignment of such NIR transitions.

9 illus, 42 ref

005149   AWASTHI A A, GUPTA N, SIDDIQUI Q T, PARAB P, PALIT D K, BOSE S, AGARWAL N (Mumbai Univ, Mumbai- 400 098, Email: sangita@cbs.ac.in) : Synthesis of acridone-naphthylamine derivative and its thermallyactivated delayed fluorescence studies for application in OLEDs. J Chem Sci 2019, 131(9), 94.

Acridone (acceptor) and naphthylamine (donor) based Donor-Acceptor-Donor (D-A-D) compound (1) was synthesised, characterised and its thermally-activated delayed fluorescence (TADF) properties were studied in detail. Compound 1 is fluorescent and emits in the green region (550 nm). The energy gap between the ground and the lowest excited singlet (S₁) state is estimated to be 2.55 eV. The energy gap between the CT singlet and triplet states (ΔE_ST) was found to be _˜ 0.3 eV. Small ΔE_S1-T1 is one of the important criteria for TADF to take place in a molecule and thus detailed photophysics has been studied. Transient lifetime measurements showed an increase in the fluorescence lifetime (s) on purging with N₂, as compared with that in air-saturated solution, indicating the involvement of the triplet state in emission. Emission at 550 nm was also observed with a delay of 100 µs which corresponded to the delayed fluorescence in 1. The lifetime of TADF was found to be 176 µs. Applications of TADF materials in organic lightemitting devices (OLEDs) has gotten attention as TADF materials utilise the triplet excitons which helps in increasing internal quantum efficiency of device. Air-saturated based on 1 were fabricated and their intensity was found to be nearly as high as 17,000 Cd/m² at 25 mA/cm² which was comparable to many of the known TADF emitters.

5 illus, 2 tables, 34 ref

005154   CHOURYAL Y N, SHARMA R K, ACHARJEE D, GANGULY T, PANDEY A, GHOSH P (Chemistry Dep, Dr. Harisingh Gour Univ, Sagar- 470 003, Email: pushpalghosh27@gmail.com) : Influence of ionic liquids and concentration of red phosphorous on luminescent Cu₃P nanocrystals. J Chem Sci 2019, 131(9), 93.

Highly crystalline, phase pure Cu₃P nanocrystals (NCs) have been successfully synthesized using ionic liquid-assisted solvothermal method at relatively low temperature (200 °C). Herein, ionic liquids (ILs) are used as a structure directing/templating agent. Effect of ILs and precursor concentration on crystal phase, crystallite size, lattice strain, morphology and grain size of Cu₃P NCs is studied. In the presence of IL, crystallite size and lattice strain significantly change with changing the concentration of red phosphorus. For example, smaller crystallite size (38.5 nm) and compressive lattice strain are obtained when 10 times of red phosphorous is used. However, bigger size (41.9 nm) and tensile lattice strains are obtained for the lower concentration of phosphorous (5 times). At higher phosphorus concentration, hexagonal shaped microcrystals with prominent grain are observed. HRTEM images reveal that spherical-shaped particles on further agglomeration through Ostwald ripening process form hexagonal-shaped bigger microstructures. However, on doping the rare-earth ions (RE³⁺ = Ce³⁺/Tb³⁺) in the Cu₃P NCs show the green luminescence (at 542 nm) which is attributed to the emission of Tb³⁺ ions. To the best of our knowledge, this is the first report on rareearth doped Cu₃P nanoparticles and shows promise on the luminescence aspect of Cu₃P nanomaterials along with its already existing plasmonic and semiconducting properties.

8 illus, 1 table, 40 ref

005211   SINGH B G, DAS R P, KUNWAR A (Radiation and Photochemistry Div, Bhabha Atomic Research Centre, Mumbai- 400 085, Email: beenam@barc.gov.in) : Protein: A versatile biopolymer for the fabrication of smart materials for drug delivery. J Chem Sci 2019, 131(9), 91.

Drug delivery is a broad field which deals with the delivery of pharmaceutical compounds to the desired site with an aim to achieve maximum therapeutic effect and minimum toxicity in treating a diseased condition. To achieve the goal, a carrier system is required for controlled and sustained drug release. Polymers are an all-time favourite matrix used to control the release of drug at the desired rate. Among the polymers, the biopolymers derived from proteins are attracting considerable attention due to their utility in delivering vaccine and chemotherapeutics in clinical application. Additionally, they are biocompatible, biodegradable, and in certain cases, cost-effective. The review addresses the source, structure and characterization of different proteins used as drug delivery carriers. Along with this, the factors contributing to the release of drug from the protein carrier has also been discussed.

2 tables, 66 ref

005162   GAUTAM A, KOMAL P, SINGH R S (O. P. Jindal Univ, Raigarh- 496 001, Email: ganurag13@gmail.com) : Future demands for high field MRI diagnostic. J Chem Sci 2019, 131(9), 89.

In the near future there would be a need for a high field MRI contrast agent for the MRI diagnostic due to the several disadvantages of Gd-based complexes, such as short circulation time and decrease in efficiency at high magnetic field i.e., greater than 3 T. The lanthanide-based nanoparticle can be an alternative to these complexes due to a high density of metal ions per unit of contrast agent. The high density of the metal ions will enable the MR signal shortening usually, at lower concentrations compared to chelates that typically are used at micro-molar concentrations. Additionally, the nanoparticles would retain their relaxivity efficiency at high magnetic field greater than 3 T.

7 illus, 1 table, 28 ref

005161   ERRANDONEA D (Fisica Aplicada-ICMUV Dep, Valencia Univ, Valencia, Spain, Email: daniel.errandonea@uv.es) : Exploring the high-pressure behaviour of polymorphs of AMO₄ ternary oxides: Crystal structure and physical properties. J Chem Sci 2019, 131(9), 88.

AMO₄ ternary oxides are materials of fundamental and technological importance exhibiting a large variety of functional properties. Members of this family of compounds have multiple potential applications; for instance, as scintillators, thermophosphors, photocatalysts, and cathodoluminescence materials. Studies under high-pressure conditions are valuable for understanding the physical properties and phase behaviour of AMO₄ oxides. In particular, great progress has been achieved in the last decade towards the understanding of the pressure-effects on the structural, vibrational, and electronic properties of AMO₄ materials. Specifically, novel metastable structures with interesting physical properties have been discovered. In this article, a selection of recent results from high-pressure studies on different AMO₄ oxides will be discussed, paying particular attention to orthovanadates. Remarkable phenomena like band-gap and volume collapses as well as phonon softening will be discussed and correlated with structural changes.

8 illus, 80 ref

005163   GAYEN A L, MONDAL D, BERA D, BISWAS P, PAUL B K, BHAR D S, DAS S, NARULA R, KHURANA A K, MANCHANDA R K, NANDY P (Centre for Interdisciplinary Research and Education, Kolkata- 700 068, Email: pnandy00@gmail.com) : Effect of Cuprum metallicum potentised through both serial dilution and succussion in comparison to succussion alone on Escherichia coli bacterial system and electrical properties of poly (vinylidene fluoride‑co‑hexafluoropropylene) polymer. Indian J Res Homoeopathy 2019, 13(4), 209-18.

Homoeopathic medicines are traditionally potentized by serial dilution followed by succussion. Respective roles of these two components need to be assessed and explored for which the present study was undertaken. To compare the effect of the medicine Cuprum metallicum (Cup. met.) potentised through both serial dilution and succussion with succussion alone on selected biological and physical systems. Starting with the medicine Cup. met. at 6C, we potentized it further to 30C and 200C by serial dilution, followed by succussion (Set A). The same medicine at 6C was also potentized to 30C and 200C by using succussion alone (Set B). The antibacterial property of these two sets was compared on E. coli, a biological system and electrical properties on polymer matrix PVDF-HFP (widely used as charge separator) a physical system. Field Emission Scanning Electron Microscopy shows that the particles get more agglomerated at higher potency in Set B. Antibacterial effect of Cup. met. in Set B at 30C and 200C was observed to be more significant as compared to Set A. Effect of Cup. met. on polymer matrix in Set A varied significantly with the potency as compared to Set B wherein less beta phase crystallization was produced followed by no significant change in electrical properties. Comparison of results using the medicine Cup. met. in two experimental set ups shows that serial dilution with succussion makes an important difference between the two sets. 

8 illus, 26 ref

005182   KUMAR V, AULAKH R S, GILL J P S, BEDI J S (Guru Angad Dev Veterinary and Animal Sciences Univ, Ludhiana- 141 004) : Analyzing efficacy of milk adulteration testing kits and conventional biochemical methods prevailing in India. Vet Pract 2019, 20(2), 256-9.

Milk safety is a challenging global problem of human health concern. It denotes a condition of being protected from physical, chemical and microbiological contamination. The chemical safety of milk for various adulterants was determined by a number of qualitative analytical tests. It is important to know the detection capability of usual biochemical methods and available kits used for preservatives, neutralizing, diluting, thickening and non-dairy fat emulsifying agent to get aware all stake holders and regulatory agencies. Laboratory investigation revealed that the analytical sensitivity of most of studied kits and methods to recognize milk adulteration were up to pph (%) level. Only the formaldehyde and water (nitrate) tests confirmed low level of fraud and able to determine the tested concentrations up to ppm level. Other tests showed limitations in detecting the unlawful addition of adulterants at tracer amount and they may not be able to assure the complete absence of these substances in milk. Moreover, a number of variants were available for a particular qualitative test used in practice. Variation in amount of chemicals used in preparation, amount of reagent used in performance, variation in test procedure were also evident in different kits and methods. Therefore, there is an immediate need for development of rapid, easy and sure tests for detection of nature and extent of adulteration, uniform monitoring to regulate milk fraud and to ensure safe and wholesome milk to consumers.

2 tables, 18 ref

005166   GUPTA V, SINGH P, KANT V, SHARMA M (Chemistry Dep, Jammu Univ, Srinagar, Jammu & Kashmir, Email: vijayta1gupta@gmail.com) : In vitro assessment of antioxidant activity, antibacterial potentials and stability of copper oxide nanoparticles. Vet Pract 2019, 20(2), 246-50.

In present study, copper oxide (CuO) nanoparticles were synthesized by chemical method and in vitro evaluated for antioxidant and antimicrobial activities. The suspension of different concentrations of CuO nanoparticles were evaluated for different parameters on day 1, 30 and 60 after its preparations. The CuO nanoparticles synthesized in this study were of 160.6 nm average size with a polydispersity index of 0.521. The CuO nanoparticles scavenge the free radicals in concentration dependent manner. The per cent inhibitions and IC₅₀ values of CuO nanoparticles against of free radicals were more and less, respectively on day 1 as compared to day 30 and 60. There were no marked reductions in the antioxidant and antibacterial actions of CuO nanoparticles suspensions on storage for 60 days. The CuO nanoparticles showed antibacterial actions against S. aureus and E. coli bacterial strains. Values of MIC and MBC of CuO nanoparticles also showed the action of CuO nanoparticles was more against E. coli than S. aureus. In conclusions, these potentials of CuO nanoparticles can be exploited to counter the diseases/problems associated with free radicals and bacteria in different fields like Veterinary and Medical sciences, agriculture, food sciences, tap water and waste water disinfection etc.

1 illus, 2 tables, 23 ref

005177   KUMAR K, ZAKIR M (Regional Research Institute of Unani Medicine, Bhadrak- 756 100, Email: kkcdri@gmail.com) : Future prospects of fermentation in Unani based drugs. Indian J Biochem Biophys 2019, 56(5), 347-51.

Unani system of medicine is being practiced in India for hundreds of years for treating various ailments by its holistic approach with natural means and drugs. Unani formulations are based on herbal, mineral and animal origin. Till date, there is no major development in different forms of the drugs and are being used as they are mentioned in the classical literature. There is need of the hour to devise pharmaceutical processing techniques to achieve palatability, more stability, absorption and assimilability of both single and compound Unani drugs without deviating from the original essence as described in the literature. Fermentation (Takhmīr) may be explored as a unique tool for the modification of dosage forms for herbal Unani drugs. It is a process of chemical change caused by organisms or their products for transformation to another compound of medicinal value. It extracts a wide range of active ingredients from the herb than any other methods of extraction. During fermentation, undesirable molecules like sugars are removed from plant extracts and made the product more bio-available and stable, less toxic and more efficient. In the Unani system of medicine, various products have been mentioned in classical literature where the process of the fermentation is applied for the preparation of drugs like Sirka, Nabeez, Dar Bahra, etc. Fermentation based drugs used in Ayurveda are Asvas and Arishthas are generally found superior to extracts for absorption in the gut with enhanced therapeutic properties, quicker action, and longer shelf life. In order to achieve better therapeutics in Unani Drugs, the process of development of compound formulation based on fermentation should be adopted for different forms of Unani formulations.

1 illus, 2 tables, 40 ref

005190   MUHAMMAD B Y, SHABAN N Z, ELRASHIDY F H, GHAREEB D A (Biochemistry Dep, Alexandria Univ, Alexandria- 21500, Email: rabbanimuhammad1@gmail.com) : Antioxidant, anti-inflammatory, antiproliferative and antimicrobial activities of Combretum glutinosum and Gardenia aqualla extracts in vitro. Free Radic Antioxid 2019, 9(2), 66-72.

Plants represent a diverse template that could be tapped as sources of novel drugs. This study highlights antioxidant, anti-inflammatory, anti-proliferative and as well anti-microbial activities of Combretum glutinosum (BE) and Gardenia aqualla (GE) roots ethanol extracts. The Biological activities were evaluated using the established standard methods. Both extracts exhibited antioxidant and anti-inflammatory activities with BE being better than GE. Anti-proliferative (cytotoxicity) assay on HepG2 and BHK-21 cell lines similarly revealed that BE (IC₅₀: 55, SI: 1.81) is more cytotoxic and more selective than GE (IC₅₀: 478.60, SI: 0.99). For the antimicrobial study, BE inhibited the growth of pathogenic bac-teria; Pseudomonas aeruginosa, Staphylococcus aureus, Vibrio species and E. coli, while GE extract showed activity against Candida albicans. We conclude that Combretum glutinosum extract (BE) possessed the most robust activity from this study. Hence, it could be a promising source of novel drug with wide biological activities, especially antioxidant and anticancer activities.

5 illus, 1 table, 33 ref

005192   NWEZE C C, DINGWOKE E J, ADAMUDE F A, NWOBODO N N (Biochemistry Dep, Nasarawa State Univ, Nasarawa, Nigeria, Email: chibuzoihe@gmail.com) : Phytochemical profile and comparative anti-radical scavenging activities of N-hexane extracts of indigenous Zingiber officinale and Curcuma longa. Free Radic Antioxid 2019, 9(2), 58-65.

The therapeutic and nutritional values of plants and plant produce for aliment management and as food supplements are evolving. Free radical scavenging activities of n-haxane extracts of indigenous Curcuma longa and Zingiber officinale was investigated and compared to CellGevity^®; a nutraceutical antioxidant supplement. In addition, their phytochemical profile was qualitatively and quantitatively determined using standard procedure for phytochemical analysis. The antioxidant activities of the extracts were determined spectrophotometrically. We used 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical, 2,2’-Azino-bis3-ethylbenzothialine-6-sulfonic acid (ABTS) radical cations and hydrogen peroxide (H2O2) to determine free radical scavenging activities of the extracts. The ability of the extracts to scavenge free radicals was determined following the discoloration of the solution mixtures, measured spectrophotometrically. The reducing power efficacy of the extracts was determined by their ability to reduce Fe³+ to Fe²+ ions. Curcuma longa and Zingiber officinale have more free radical scavenging power compared to CellGevity^®. Curcuma longa has more scavenging power against DPPH and H₂O₂ system, while Zingiber officinale has more scavenging power against ABTS cations. CellGevity^® had the least scavenging activity against the free radicals, as observed in this study. The highest phenolic, flavonoid, Vitamin C, Vitamin B₁ and Vitamin B₂ quantified were found in Curcuma longa and Zingiber officinale compared to CellGevity^®. The indigenous Curcuma longa and Zingiber officinale are natural sources of effective antioxidants with more scavenging power compared to a standard CellGevity^® nutraceutical.

2 illus, 5 tables, 59 ref

005174   KIM S-J, LEE S, BANG E, LEE S, RHEE J-K, NA Y-C (Korea Basic Science Institute, Seoul- 03759, Email: nyc@kbsi.re.kr) : Comparative evaluation of flavor compounds in fermented green and roasted coffee beans by solid phase microextraction‐gas chromatography/mass spectrometry. Flavour Fragr J 2019, 34(5), 365-76.

Specific fermentation processes such as digestive bioprocessing and monsooning have been of interest to coffee consumers. Volatile compounds of beans during the different fermentation processes vary considerably and exhibit different profiles. The representative flavor compounds for the luwak green bean were found to be pentamethyl heptane and 3‐methyl‐1‐butanol, while more diverse and distinct compounds were observed from the monsooned green bean, namely alkyl butanals, pinenes, benzaldehyde and butanediols. However, after roasting, the fermented form of both beans contained similar types of volatiles and their relative contents compared to those of non‐fermented roasted beans, except for α‐pinene in luwak and 2‐methyl furan in monsooned beans. In principal components analysis and partial least squares‐discriminant analysis (PLS‐DA), the different fermented beans were clearly distinguished by the extracted peak entities from their total ion chromatograms. The s‐plot and variable importance on projection (VIP) values related to PLS‐DA showed the significant compounds contributing to the identification of the groups. 3‐Methyl‐1‐butanol was the most distinctive compound for the luwak green bean, and β‐pinene, ethylbenzene and benzaldehyde were found to be the significant compounds in the monsooned green bean. In roasted beans, the most significant compounds to distinguish luwak were furfural, α‐pinene and 3‐carene with high variable in the projection (VIP) values. A significant presence of pyrazine, alkyl pyrazines, pyridine and alkyl pyridines contributed to differentiating both fermented roasted coffee beans from the unfermented roasted beans.

4 illus, 4 tables, 36 ref

005147   ARIGO A, RIGANO F, MICALIZZI G, DUGO P, MONDELLO L (Chemical, Biological, Pharmaceutical and Environmental Sciences Dep, Messina Univ, Messina- 98168, Email: Imondello@unime.it) : Oxygen heterocyclic compound screening in Citrus essential oils by linear retention index approach applied to liquid chromatography coupled to photodiode array detector. Flavour Fragr J 2019, 34(5), 349-64.

To date, liquid chromatography coupled to a photodiode array (PDA) detector is the main technique employed to analyse furocoumarins (FCs) in essential oils. This type of detection may lead to poor performance because of the low sensitivity and se-lectivity of PDA detection. In this work, the linear retention index (LRI) was used in combination with a UV-Vis library for the identification of 35 oxygen heterocyclic compounds in Citrus essential oils, making it possible to distinguish compounds with very similar spectra. As opposed to retention time, which can significantly change with the instrument or laboratory used, LRI represents a kind of normalized relative retention time, as independent as possible from operating conditions. From a qualita-tive point of view, reproducibility results are provided to definitively assess the suit-ability of such an approach for inter-laboratory use and for a fully automated process, even when pure and very expensive standard materials are not available, as just the LRI database and the UV-Vis library are needed. From a quantitative point of view, calibration curves were created in pure solvent and by adding standard compounds to several blank matrices, with the aim of evaluating differences, overcoming matrix effects, achieving the correct limits of quantification, and providing the quantita-tive profile of real samples. The LRI system is not listed in the Commission Decision 2002/657/EC as criteria for the Full Scan UV-Vis detection; however, its validity and applicability are here investigated and proposed for future applications, in combina-tion with the UV-Vis library.

4 illus, 4 tables, 47 ref

005215   SRIVASTAVA M (Chemistry Dep, DBS (PG) Coll, Dehradun, Email: dr.mahima@hotmail.com) : Additives: A boon to new age industry. Everyman's Sci 2019, 54(3), 155-9.

Additives are compounds added to enable desired balance of properties to be achieved for any particular application. The use of such ingredients, commonly stated as additives, has played an essential role in the commercial development of base materials. They are used for a variety of purposes: to improve processing, modify performance or appearance, prevent or retard aging and to reduce cost. This article covers and discusses the most active heterocycles that have shown considerable actions such as stabilizers, preservatives, surfactants, retardants, curatives, accelerators, etc.

10 ref

005151   BAGHEL A, BHUVANESWARI A, SINGH V V, BOOPATHI M, SINGH B (DRDO- Defence Research and Development Establishment, Gwalior- 474 002, Email: anubaghl@drde.drdo.in) : Synthesis and characterization of ligand free cadmium imprinted polymer for sensing of Cd(II) from aqueous solution. Def Life Sci J 2019, 4(3), 153-7.

Cadmium(II)-imprinted polymer [Cd(II)-IIP] was synthesised without using the conventional complexing ligand to  reduce  unnecessary  step  for  complexing  Cd(II).  During  synthesis  of  Cd(II)-IIP,  the  complete  removal  of  Cd(II) from the polymer was confirmed using Energy Dispersive Analysis of X-rays (EDAX) and Atomic Absorption Spectrophotometer  (AAS).  Synthesised  polymers  ([Cd(II)-IIP],  non-imprinted  polymer  (NIP)  and  polymer  with cadmium  (CdP)  were  also  characterised  and  compared.  Scanning  electron  microscope  (SEM)  analysis  of  Cd(II)- IIP indicated the changes in surface morphology after imprinting, the polymer looked like a flaky material in comparison  with  NIP  and  CdP.  BET  surface  area  of  Cd(II)-IIP  (68m² /g)  was  found  to  be  more  than  that  of  NIP  (24.6m²   /g)  and  CdP  (17m²  /g).  Cd(II)-IIP  formed  a  complex  with  Cd(II)  in  the  solution  through  carbonyl  oxygen of the acrylamide as confirmed by FTIR. TGA analysis showed less char yield for Cd(II)-IIP than NIP. Cd(II)-IIP was further explored for the fabrication of ion selective electrode (ISE), which on binding with Cd(II) gave higher potential  than  NIP-ISE.  Interference  study  was  also  performed  using  Cd(II)-IIP  as  such  and  also  with  fabricated ISE with Cd(II)-IIP using different cations such as Pb(II), Zn(II), Mn(II), Hg(II), and found that imprinted polymer showed  more  selectivity towards  Cd(II)  in  aqueous  solutions.

4 illus, 1 table, 18 ref

005167   HARSHADA L, MADHURI D, RAJKUMAR S, RAHUL S (Pharmaceutics Dep, R.D. Coll of Pharmacy, Maharastra- 412 206, Email: harshada.lawale2015@gmail.com) : Formulation and evaluation of celecoxib solid dispersion. Int J Pharm Biol Sci 2019, 9(3), 21-31.

The purpose of present study is to develop stomach specific celecoxib solid dispersion using eudragit EPO as a carrier for enhancing solubility as well as rate in gastric environment. Enhanced dissolution rate and solubility in gastric pH was achieved by formulating celecoxib solid dispersion by hot melt extrusion techniques. The celecoxib solid dispersion prepared by 2² factorial design. The drug and eudragit EPO in different ratios like 1:1,1:2,1:3 and 1:4 were used for formulating solid dispersion. FTIR spectra of celecoxib in alone and combination showed compatibility of drug and excipient. The solid dispersion was evaluated for percentage yield, drug content and percent drug release and results found to be 97.50 %, 99.43 % and 87.97 % respectively. Stability study was performed in closed container at 30 ^oC ± 2 ^oC/65% RH ± 5% RH and 40 ^oC ± 2 ̊C/75% RH ± 5% RH. It was concluded that 1:1 ratio of celecoxib solid dispersion shows better in-vitro dissolution rate as compared to pure drug The increased dissolution rate of celecoxib solid dispersion in gastric pH was attributed to the effect of eudragit EPO which was clearly shown by SEM, DSC and P-XRD studies.

12 illus, 8 tables, 24 ref

005181   KUMAR T H, BEGUM A, SANKAR D G (Pharmaceutical Analysis and Quality Assurance Dep, Vignan Institute of Pharmaceutical Technology, Visakhapatnam, Andhra Pradesh) : Determination of Azilsartan Medoximil and Chlorthalidone in tablets exposed to forced degradation by using RP-HPLC. Biomed Res 2019, 30(5), 775-85.

An RP-HPLC method was developed which was simple, specific and precise accurately and was validated for the simultaneous estimation of Azilsartan Medoxomil and Chlorthalidone by following forced degradation studies in pharmaceutical formulation. The method has been developed using Enable C 18G column (250 × 4.6 mm, 0.5 µm) and a mobile phase comprising of acetonitrile and 0.1 % trifluoroacetic acid in water at the ratio of 40:60 %v/v with a flow rate of 0.8 mL/min. UV detection was carried out at 240 nm. The retention time for Azilsartan Medoxomil and Chlorthalidone were found to be 6.982 and 7.748 min respectively. The proposed method was validated for various parameters like linearity, range, accuracy, precision, robustness, LOD and LOQ. Linearity was observed over a concentration range 5-80 µg/ml for Azilsartan Medoxomil (r²=0.9995) and 2.5-25 µg/ml for Chlorthalidone(r²=0.9973). The % RSD for Intraday and Interday precision was found as 0.41 and 0.41 for Azilsartan Medoxomil and 0.32 and 0.47 for Chlorthalidone respectively. The LOD and LOQ were found as 0.0189 µg/ml and 0.0305 µg/ml for Azilsartan Medoxomil and LOD and LOQ were found to be 0.1109 and 0.3522 µg/ml for Chlorthalidone respectively. Azilsartan Medoxomil and Chlorthalidone have been subjected to stress conditions of degradation including acidic, alkaline, oxidative, and thermal and photolysis.

10 illus, 11 tables, 26 ref

005197   PERVEEN S, ORFALI R, AL-TAWEEL A M, KHAN A, ALGHANEM B, SHAIBAH H (Pharmacognosy Dep, King Saud Univ, Riyadh, Saudi Arabia) : Simultaneous identification of phenolic and flavonoid contents in bee pollen by HPLC-ESI-MS data. Biomed Res 2019, 30(5), 770-4.

A HPLC-MASS method has been developed for the characterization of secondary metabolites present in the methanol extract of honey bee pollen pallet. As a result, three new and five known compounds were identified or tentatively characterized by using ESIMS data. The chemical composition of methanol extract of pollen pallet is presented for the first time by using the LC-ESI-MS method. In conclusion, LC-MS/MS based chemical screening of diverse bioactive compounds in matrices of bee pollen pallet methanol extract would appear to be an effective approach for discovering new/known compounds. A high percentage of the detected compounds corresponded to glycosylated flavonoids and phenolic were identified.

9 illus, 1 table, 9 ref

005152   BALOCH R, UZAIR M, CHAUHDARY B A, HAYAT M M, ALAMGIR M (Bahauddin Zakariya Univ, Multan, Pakistan) : Phytochemical analysis, antioxidant and cytotoxic activities of Dryopteris ramosa. Biomed Res 2019, 30(5), 764-9.

The aim of present study was to evaluate phytochemical, cytotoxic and antioxidant potential of dichloromethane and methanol extracts of Dryopteris ramosa (Hope) C. Chr. belongs to family Dryopteridaceae. The plant is traditionally used as anthelminthic, diuretic, antibacterial, astringent and as tonic for various stomach and intestinal problems. The phytochemical potential, total phenol, flavonoid and alkaloid contents of Dryopteris ramosa were determined for the first time. Plant was subjected to Brine shrimp lethality and DPPH inhibition assay was done. Identification and quantification of various phenolic content by was done HPLC. Phytochemical analysis revealed that flavonoids, terpenoids, cardiac glycosides, alkaloids and saponins were present in the plant while tannins were absent. The results depicted high in vitro cytotoxic effect by dichloromethane extract with a LD₅₀ 0.6903 µl/ml as standardized with Etoposide with LD₅₀ of 7.4625 µl/ml. The methanol extract showed the strong DPPH scavenging activity with 72.76 ± 1.52 % inhibition as compared to the dichloromethane extract with 55.37 ± 3.055 % inhibition. The high phenol content was found in methanol extract having 199.2 ± 4.50 (mg of GA/g of extract). HPLC analysis showed the presence of various phenol compounds (Gallic acid, quercetin, caffeic aid, vanillic acid, cinnamic acid etc.) with their relevant concentration, in the plant. The dichloromethane extract exhibited high flavonoid content 73.02 ± 1.00 (mg of RE/g of extract). Alkaloidal content was highest in dichloromethane extract with 29.73 ± 4.04 (mg of AE/g of extract).

2 illus, 6 tables, 25 ref

005207   SANTHOSHAKUMARI T M J, SNEHA M (Biochemistry Dep, Sri Lakshmi Narayana Institute of Medical Sciences, Puducherry, Tamil Nadu) : Association between abdominal obesity and subclinical hypothyroidism. Biomed Res 2019, 30(5), 760-3.

Abdominal obesity or increase in waist circumference is one of the important components of metabolic syndrome. In this study the association between waist circumference (abdominal obesity) with subclinical hypothyroidism (SCH) was analysed. To identify patients with and without abdominal obesity. To assess the association between subclinical hypothyroidism and abdominal obesity in these two groups.  75 subjects with abdominal obesity and 75 with normal Waist circumference (WC) were enrolled and BMI, Blood pressure (BP) and serum free T3, free T4, and TSH were done. Base line characteristics of the study participants are expressed as Mean ± SD and percentage. The difference in anthropometric and biochemical parameters in the study group and control group was analysed by student‘t’ test. In the study group 55 subjects (73 %) were euthyroid, 20 subjects (27 %) had subclinical hypothyroidism. Interestingly in the control group 66 subjects (88 %) were euthyroid, 9 subjects (12 %) had subclinical hypothyroidism. This shows that in our study abdominal obesity and SCH have statistically significant association.

3 tables, 25 ref

005194   PANT A, JHA K, AGARWAL S, KAUR H, SINGH M (Biotechnology Dep, Jaypee Institute of Information Technology, Noida, Uttar Pradesh, Email: manishasingh1295@gmail.com) : Fabrication, validation, and stability analysis of Melaleuca alternifolia oil-in-water microemulsion for improved transdermal application. Asian J Pharm 2019, 13(3), 252-65.

The aim of the study was to develop oil-in-water microemulsion (ME) system for Melaleuca alternifolia for targeting skin disorders. The formulation of ME system was done through the water titration method, which involved various oils, water, surfactants, and cosurfactants. The existence zones of ME were determined by constructing ternary phase diagrams, where surfactants and cosurfactants (S_mix) were taken in different ratios along with different combinations of oil and S_mix. Quantitative estimation of tea tree oil (TTO) was performed using gas chromatography-mass spectrometry followed by total terpenoid estimation, and thereafter, solubility studies of TTO were performed using various excipients. TTO-ME was fabricated and characterized using modern characterization techniques (DLS, transmission electron microscopy, and Fourier transform infrared) along with statistical validation and in vitro drug release assessment. The optimized TTO loaded MEs (TTO ME) showed the particle size range between 32 and 160 nm with poly dispersibility index of 0.297 and zeta potential of −3.19 mv with almost spherical morphology. The optimized formulation showed the sustained release of the therapeutic compound and was found to be stable at room temperature for 1 year, suggesting being a promising formulation against dermal infections. TTO was successfully loaded in thermodynamically stable ME system which enhanced its permeation through the transdermal route. Therefore, a novel drug delivery system was introduced, which can be studied on various in vitro and in vivo models further to establish its better therapeutic efficacy for various skin disorders.

9 illus, 11 tables, 52 ref

005189   MOGLAD E H O, ALHASSAN M S, ABDALKAREEM E A, ABDALLA A N, KUSE M (Pharmaceutics Dep, Prince Sattam Bin Abdulaziz Univ, Alkharj- 11942, Email: ehssanhassn@yahoo.com) : Ethyl acetate fraction of Solanum nigrum L.: Cytotoxicity, induction of apoptosis, cell cycle in breast cancer cells, and gas chromatography-mass spectrometry analysis. Asian J Pharm 2019, 13(3), 246-51.

The objective of this study was to evaluate the cytotoxic, apoptotic, and cell cycle effect of four fractions obtained from the whole aerial part of Solanum nigrum, against three cancer cell lines (MCF-7, A2780, and HT29) and one normal cell line (MRC-5). MTT assay was used to assess the cytotoxicity of the four fractions. Then, the most active fraction (ethyl acetate) was further examined by annexin V propidium iodide (PI)/FITC apoptosis assay, cell cycle analysis in MCF7 cells followed by gas chromatographymass spectrometry (GC-MS) analysis. The highest growth inhibition activity was obtained by the ethyl acetate fraction (IC₅₀ 10–12 µg/ml) against the three cell lines and that fraction spared the normal cell line MRC5 with IC₅₀ of 31.78 µg/ml. Annexin V PI/FITC revealed a dose-dependent induction of apoptosis in MCF7 cells when treated the ethyl acetate fraction; which also caused a non-dose dependent S phase arrest. The GC-MS analysis of the ethyl acetate fraction showed fatty acids and esters of fatty acids as the significant components. The ethyl acetate fraction from S. nigrum strongly inhibited the growth of breast, ovarian, and colon cancer cell lines, and it was three folds selective against the normal fibroblasts. It also caused the induction of early apoptosis and S phase cell cycle block at 10 µg/mL. Future bioassay-guided fractionation of the ethyl acetate fraction could reveal the active compounds, which can be more investigated in further studies.

2 illus, 3 tables, 34 ref

005219   THAKUR S, SINGH B, VYAS M, SAINI G, YADAV R S, KHATIK G, CHAUDHARY A, SHARMA N (Ayurveda Dep, Lovely Professional Univ, Phagwara- 144 411, Email: vymanish@gmail.com) : Development of analytical method and its validation in bilayer tablet containing fexofenadine hydrochloride (Immediate Release Layer) and montelukast sodium (Sustained Release Layer). Asian J Pharm 2019, 13(3), 238-45.

The aim of the present study was to develop and validate the analytical method for bilayer tablets. Simultaneous estimation of fexofenadine hydrochloride (HCl) and montelukast sodium in bilayer tablets by ultraviolet spectrophotometric method. The absorption maxima of fexofenadine HCl and montelukast sodium were found to be 259 nm and 285 nm, respectively, using phosphate buffer pH 6.8. The method obeys Beer’s law in the concentration range of 24–84 µg/ml and 2–14 µg/ml for fexofenadine HCl and montelukast sodium, respectively. Different analytical parameters such as limit of detection, limit of quantitation, accuracy, and precision were determined as per International Council for Harmonisation guidelines Q² (R¹). The accuracy of the method was found to be 99.71 % and 99.13 % for fexofenadine HCl and montelukast sodium, respectively. There is no interference shown by the excipients of the formulation in the method and the method can be used for routine quality control.

6 illus, 9 tables, 12 ref

005205   RUHELA A, VYAS M, YADAV P, KHATIK G L, GALIB, PRAJAPATI P K, KHURANA N, SHARMA N (Rasashastra and Bhaishajya Kalpana Dep, All India Institute of Ayurveda, New Delhi- 110 076, Email: drpramod88@gmail.com) : Stability study of Bhallataka kshaudra: An ayurvedic formulation. Asian J Pharm 2019, 13(3), 233-7.

Bhallataka (Semecarpus anacardium L.), commonly known as “marking nut,” has vast applicability in indigenous system of medicine and is indicated in many ailments such as skin disorders, tumors and malignant growth, fungal disease, excessive menstruation, vaginal discharge, fever, hemoptysis, constipation, and intestinal parasites. About 40 formulations of Bhallataka are mentioned in Bharat Bhaishajya Ratnakar. Acharya Charaka has described ten different formulations of Bhallataka in Rasayana Adhyaya. Bhallataka Kshaudra is among the 10 Kalpana of Bhallataka. The ratio of Kshaudra (Honey):Bhallataka oil: Ghrita (Ghee) is 1:8:16, respectively, for the preparation of Bhallataka Kshaudra. The stability study is carried out to establish the duration of shelf life of the product under specified storage condition. Accelerated stability study was carried out under atmospheric condition temperature: 40 ± 2°C and relative humidity: 75 ± 5 %. Organoleptic parameters, physicochemical parameters, microbial limits, and heavy-metal analysis were observed studied during the study. No significant change was observed in any of the parameters observed during the stability study. Based on the stability data, the shelf life expected to be 4.49 years. The extrapolated shelf life of Bhallataka Kshaudra is found to be 4.49 years on assessing the analytical parameters. The microbial count and heavy metals were within permissible limits.

3 illus, 7 tables, 6 ref

005198   PRASANTHI N L, HARSHITA Y, MANIKIRAN S S, RAMARAO N (Pharmaceutics Dep, Chalapathi Institute of Pharmaceutical Sciences, Guntur, Andhra Pradesh, Email: prasanthi_pharm@yahoo.com) : Design and development of gastroretentive tablets of Coccinia grandis leaf extract for treating Helicobacter pylori infection. Asian J Pharm 2019, 13(3), 184-91.

To design and develop a gastroretentive herbal formulation of Coccinia grandis for the treatment of Helicobacter pylori infection. C. grandis extract was obtained by soxhlation process with ethanol as the menstrum. The herbal gastroretentive tablets containing 200 mg of C. grandis ethanolic extract were prepared by direct compression method using effervescent technique. HPMC K4M, HPMC K100M, Carbopol and guar gum were used as retarding polymers at various concentrations. Sodium bicarbonate was used at 20 % w/w as gas generating agent and Avicel at 35 %w/w as diluent. FTIR and DSC methods were employed to investigate the drug-excipient interactions. The formulated tablets were evaluated for various quality control parameters. The FTIR and DSC study revealed that there was no interaction between the extract and the excipients. All the formulated tablets were within the quality control limits. The kinetic studies specified that the release of extract from the gastroretentive tablets was by erosion-controlled diffusion mechanism. The formulation having the combination of gum with HPMC K15M exhibited minimum floating lag time and good release pattern which followed first-order kinetics.

3 illus, 5 tables, 23 ref

005200   PRIYA K K, ANURADHA V (Chemistry Dep, Vignan Degree Coll, Guntur- 522 004, Email: kavi_kkp@yahoo.co.in) : A novel pyridyl ester isolated from Leucas cephalotes. Asian J Chem 2019, 31(10), 2410-2.

From the flowers of Leucas cephalotes, pyridine-3-carboxylic acid ester was isolated. Its structure was established as 2′,5′-dihydroxy-3′- pyridyl-(2,5-dihydroxy)pyridinyl-3-carboxylate on the basis of spectroscopic analysis. To out best of knowledge, this is the first report from Leucas cephalotes in particular and Labiatae family in general.

2 illus, 30 ref

005209   SIDDIQUE M N I, ZAIED B K, KRISHNAN S, AHMAD M F (Malaysia Terengganu Univ, Kuala Nerus- 21030, Email: m.nurul@umt.edu.my) : Improving methane generation by co-digestion of sewage sludge and petrochemical wastewater: Influence of heat and alkali pretreatment. Asian J Chem 2019, 31(10), 2403-9.

With the target of amplifying methane generation from sewage sludge (SS), co-digestion with petrochemical wastewater (PWW) was examined. In addition, the use of both 165 °C heat treatment and alkali pretreatment to mixed SS/PWW wastewater was assessed. Batch tests demonstrated that refractory materials were generated from pretreatment for petrochemical wastewater at the 165 °C heat and alkali pretreatments at the 75 or 115 °C and with pH value of 8, 9 or 10 producing enhanced preliminary methane generation percentage and a little effect for generation capacity of methane of the miscellaneous waste (+3–6 %). Anaerobic reactors which were operated more than four months semi-continuously with sewage sludge and petrochemical wastewater mix with the proportion of 85:15, 55:45 and 85:15 pretreated at alkaline environments maintaining the temperature of 75 °C and pH = 8. This pretreatment enhanced the production of methane at semi-continuous anaerobic reactors to + 59 %. Finally, this investigation demonstrated the viability of the co-digestion of sewage sludge with a higher ratio of petrochemical wastewater [45 % volume, 50 % volatile solid (VS) and 74 % COD, comparable with volatile fatty acids of 8 g L^–1]. The system produced an exact methane of 363 mL CH4 g^–1 VS while only sewage sludge generated 117 mL CH4 g^–1 VS.

1 illus, 6 tables, 35 ref

005172   KAUR H, SHARMA A (Chemistry Dep, Lovely Professional Univ, Phagwara - 144 411, Email: harpreet2.kaur@lpu.co.in) : Biosynthesis, anti-TB activity and degradation of dyes by silver nanoparticles using fruits peels. Asian J Chem 2019, 31(10), 2397-402.

In the present work, waste materials such as pomegranate and orange peels were taken to synthesize nanoparticles by biological method. The method did not involve the use of toxic reducing and capping agents. It uses only the environmentally benign biomolecules for reduction of AgNO₃ and subsequent stabilization of silver nanoparticles. The size of pomegranate and orange silver nanoparticles varied from 8-25 nm with nearly spherical morphology as analyzed by XRD and TEM studies. The synthesized nanoparticles were studied for their dye degrading property. Different dyes such as crystal violet, methylene blue, malachite green and Congo red were taken for the study. The results indicated the presence of two diverse mechanism of dye removal. Crystal violet, methylene blue, malachite green was removed by adsorption onto both the nanoparticles, whereas Congo red was reduced by NaBH₄ in the presence of catalytic pomegranate silver nanoparticles. Moreover, pomegranate silver nanoparticles have exhibited potent antitubercular activity with MIC value of 6.25 µg/ mL and orange silver nanoparticles are moderately active with MIC value of 25 µg/mL. It could be concluded that the pomegranate silver nanoparticles would a promising candidate for drug development and catalysis.

8 illus, 1 table, 23 ref

005210   SILIVERI S, VAMARAJU H B, SHIVARAJ (Pharmaceutical Chemistry Dep, G. Pulla Reddy Coll of Pharmacy, Hyderabad- 500 028, Email: sravanthisiliveri@gmail.com) : Synthesis and biological evaluation of furo[3,2-c]pyrazole-5-carbimidates. Asian J Chem 2019, 31(10), 2389-93.

In the present work, novel pyrazole fused dihydrofurans synthesized via a chronological addition of N-chloro succinimide and base piperidine to pyrano[3,2-c]pyrazole carbonitrile derivatives in methanol medium. Oxidative difunctionalization was done with the reagent N-chloro succinimide by the addition of both chlorine and alkoxy groups crosswise the chromene double bond. The addition of base results in the construction of dihydrofuran derivatives by ring contraction. The structures of newly synthesized compounds were characterized on the basis of physical and spectral data. Synthesized compounds were evaluated for antibacterial and anti-inflammatory activities. All the compounds exhibited significant antibacterial activity against all the four strains of bacteria and their MICs ranged between 1.56 and 12.55 µg/mL. In anti-inflammatory screening, among all the tested compounds, compounds 7, 8, 9, 11, 12, 13, 14, 16, 17 and 18 exhibited significant protection against the edema formation at a concentration of 100 mg/kg.

2 tables, 20 ref

005214   SRAVYA G, SURESH G, ZYRYANOV G V, BALAKRISHNA A, REDDY N B (Ural Federal Univ, Yekaterinburg- 620 002, Email: drbvreddyn@gmail.com) : K₂CO₃/Al₂O₃: An efficient and recyclable catalyst for one-pot, three components synthesis of α-aminophosphonates and bioactivity evaluation. Asian J Chem 2019, 31(10), 2383-8.

A simple and efficient method has been employed for synthesis of a novel series of biologically active α-aminophosphonates (4a-j) by reacting 1H-benzo[d]imidazole-2-carbaldehyde and various aromatic amines (2a-j) and diethyl/dimethyl phosphite by Kabachnik-Field's reaction in the presence of efficient heterogeneous K₂CO₃/Al₂O₃ catalyst under solvent-free conditions at 140 ºC. Structures of all the compounds were confirmed by ¹ H, ¹³C and ³¹P NMR and LC-MS. In addition to this antioxidant activity were also evaluated.

3 tables, 52 ref

005156   DESAPPAN V, VISWANATHAN J (PG & Research Chemistry Dep, Presidency Coll, Chennai- 600 005, Email: vjaisankar@gmail.com) : Synthesis and characterization of biodegradable jatropha oil based polyurethanes using modified sesame oil as cross-linker containing different NCO groups with improved thermal stability. Asian J Chem 2019, 31(10), 2375-82.

In this work, the modified S-diol were prepared from sesame oil to produce polyol. The thermal responsive vegetable oil-based polyurethane was prepared by polycondensation method. The different diisocyanate react with jatropha-sesame oil polyol to produce higher density with molecular weight of polyurethanes structure and functionality were characterized by Fourier transform spectroscopy, proton nuclear resonance spectroscopy and gel permeation chromatography. The thermal analysis was carried with TG analysis. The kinetic and thermodynamic parameters was calculated by TGA decomposition temperature and compared with PU-1, PU-2 and PU-3. Furthermore, the corresponding decomposition temperature of polyurethanes activation energy were calculated by Coats-Redfern, Sharp-Wentworth and Freeman-Carols methods, and it is investigated with lifetime of polyurethanes. Depending on the physically observed NH and C=O linkages of polyurethane matrix, which enhancing the hard and soft segment to improve their chain mobility. The success of the investigated polyurethanes, the corresponding estimated enthalpy, entropy and pre-exponential factors are much closer with toluene and phenyl based polyurethane matrix.

5 illus, 3 tables, 31 ref

005184   LIU E, JIAN F (Henan Univ of Science and Technology, Henan Province, P.R. China, Email: ffj2017@haust.edu.cn) : Crystal structure and electrochemical property of tetrazole complex of copper [Cu(pta)₂(NO₃)₂(H₂O)₂] (pta = 1-phenyl-1H-tetrazole). Asian J Chem 2019, 31(10), 2370-4.

A new compound, [Cu(pta)₂(NO₃)₂(H₂O)₂] (pta = 1-phenyl-1H-tetrazole) has been synthesized and characterized by IR, elemental analysis and single-crystal X-ray diffractions. X-ray structural analysis reveals that each Cu atom is coordinated by two pta molecules, two nitrate ions and two water molecules to form octahedral coordination geometry. O(1w) atoms of the water molecules serve as H-donor to interact with the nitrate oxygen atoms O(2), O(3) (H-acceptor) and form 1D hydrogen-bond ladder chains. These chains then, construct a 2D network layer via π-π stacking interactions between the five-membered ring of tetrazole and the six-membered ring of benzene. The 3D framework was constructed through the hydrogen bonds of C(7)-H(7A)····O(3). The behaviour of cyclic voltammetry of the compound on three-electrode cell showed an irreversible process.

6 illus, 4 tables, 26 ref

005208   SHOOTO N D, NAIDOO E B (Chemistry Dep, Vaal Univ of Technology, Vanderbijlpark- 1900, Email: ntaotes@vut.ac.za) : Detoxification of wastewater by paw–paw (Carica papaya L.) seeds adsorbents. Asian J Chem 2019, 31(10), 2249-56.

The present work reports the biosorption studies of metal ions viz., Pb(II) and Cu(II) from aqueous solution onto paw-paw seeds (PPS), acid treated paw-paw seeds (ATPPS) and base treated paw-paw seeds (BTPPS) adsorbents by batch method. A series of tests were carried to evaluate the effect of the system parameters, i.e. adsorbent dosage, initial concentration, temperature and contact time. The obtained kinetic data showed that the pseudo first order model best fitted the biosorption of both metal ions with (r² ) values of 0.9918, 0.9674 and 0.9463 for Cu(II) onto PPS, ATPPS and BTPPS, respectively and for Pb(II) 0.8513, 0.8686 and 0.9434 onto PPS, ATPPS and BTPPS respectively. Estimated surface adsorption of intra-particle diffusion estimated that surface sorption dominated. Thermodynamic parameter (∆G^o) gave negative values indicating that the biosoption processes were spontaneous and feasible. ∆H^o gave positive and negative values indicating that some biosorption processes were endothermic and some exothermic. Isotherm data indicated that Langmuir best described the biosorption. The reusability of PPS, ATPPS and BTPPS adsorbents was evaluated up to five cycles without showing significant drop in sorption efficiency.

9 illus, 5 tables, 32 ref

005171   KAUR A P, GAUTAM D (Chemistry Dep, Sant Baba Bhag Singh Univ, Jalandhar-144 030, Email: dpkgtm641@gmail.com) : Ultrasound aided expedient synthesis, characterization and antimicrobial studies of fluorenyl-hydrazono-thiazole derivatives. Asian J Chem 2019, 31(10), 2245-8.

Ultrasound assisted facile synthesis of fluorenyl-hydrazonothiazoles (4a-d) in quantitative yields by the condensation of 2-(9H-fluoren9-ylidene)hydrazinecarbothioamide (2) with substituted phenacyl bromides in presence of dimethyl formamide has been reported. The reaction of carbothioamide 2 with α-haloacids resulted in to fluorenyl-hydrazonothiazolidin-4-ones (3). The structural characterization of the cyclized products have been established by elemental analysis and spectral data (IR, NMR and mass). The antimicrobial studies of the synthesized compounds are also reported.

2 tables, 17 ref

005196   PATEL V, PATEL A A, DIXIT B, DIXIT R (Pharmaceutical Chemistry Dep, Sardar Patel Univ, New Vallabh Vidyanagar- 388 120, Email: ritsdixit@yahoo.co.in) : Simultaneous removal of dyes colour and Cu(II) metal ions using acetone-formaldehyde-salicyclic acid resin. Asian J Chem 2019, 31(10), 2240-4.

Removal of dyes colour and Cu(II) metal ion from aqueous solution using acetone-formaldehyde-salicyclic acid (AFSA) resin has been carried out. The results revealed that AFSA resin acts as a cheap substitute to commercial adsorbent like activated carbons. The effects of pH, adsorbent dose, contact time, and initial dye and Cu(II) metal ion concentration on the adsorption efficiencies were investigated. Isotherm studies were conducted using Langmuir and Freundlich models, and thermodynamic studies were also performed. Adsorption of dyes was found to obey the Langmuir isotherm model and have endothermic process. The maximum adsorption capacities calculated from the Langmuir isotherm were found to be 88.18 and 2.9 mg/g for methyl orange dyes.

13 illus, 3 tables, 16 ref

005157   DEVI P V, SUNEETHA M, RAVINDHRANATH K (Chemistry Dep, K L Univ, Vaddeswaram- 522 502, Email: ravindhranath.kunta@gmail.com) : Effective activated carbon as adsorbent for the removal of copper(II) ions from wastewater. Asian J Chem 2019, 31(10), 2233-9.

Nitric acid activated carbons prepared from the barks of Limonia acidissima plant (NALABC) and stems of Hibiscus cannabinus plant (NAHCSC) are investigated as adsorbents for the removal of Cu(II) ions from waste water using batch methods of extraction. Various extraction conditions namely, pH, time of equilibration, sorbent concentration, initial concentration of Cu(II) ions and temperature, are optimized for the maximum removal. Substantial amounts of Cu(II) are extracted in the pH range: 3 to 9 and adsorption capacities are 19.6 mg/g for NALABC and 29.4 mg/g for NAHCSC, which are more than many active carbons developed in the previous works. It is interesting to note that the adsorbents are effective in acidic, neutral and also in basic conditions of the water samples and thus paving the way for applying these adsorbents in wide pH ranges of diverse samples. Five-fold excess of common co-ions that are normally present in water, have marginally affected the % removal. Thermodynamic parameters are evaluated for the spontaneity and nature of adsorption processes. The adsorption phenomenon is analyzed using Langmuir and Freundlich isotherm models and noted that Langmuir isotherm model suits better indicating the uniform and mono-layer nature of adsorption. Kinetics of adsorption is analyzed and found that pseudo second-order kinetics preferably explains the adsorption of Cu(II). The spent NALABC and NAHCSC can be regenerated and subsequently used. The adsorbents developed are found to be effective in removing Cu(II) ions from the real water samples collected from polluted lakes and copper based industries.

7 illus, 4 tables, 29 ref

005144   ALEXANDER M, KALAIVANI R A, SRIRAMAN V, SENTHILKUMAR U (Chemistry Dep, Vels Institute of Science, Technology & Advanced Studies, Pallavaram-117, Email: chemalexander802@gmail.com) : Electro polymerization of o-phenylenediamine using palladium nanoparticles coated fabricated TiO₂ nanotubes modified glassy carbon electrode. Asian J Chem 2019, 31(10), 2229-32.

Fabricated titanate nanotubes (f-TNT) are prepared by chemical deposition method using linen fiber. The f-TNTs is fabricated by TiO₂ nanoparticles, the each TiO₂ nanoparticles diameter has 80-100 nm in range. The Pd⁰ nanoparticle was coated on the surface of the f-TNT by chemical reduction method, using NaBH₄ as reducing agent. The prepared Pd/f-TNTs characterized by FT-IR, FE-SEM and HRTEM, the result shows that the f-TNT diameter is 1500 nm and Pd nanoparticles range in 20-50 nm. The Pd/f-TNT nanocomposite modified glassy carbon (GC) electrode shows quasi irreversible redox behaviours in cyclic voltammeter. Those Pd/f-TNTs modified electrode is utilized for electrochemical polymerization of o-phenylenediamine in acid medium.

4 illus, 1 table, 26 ref

005178   KUMAR P S, KRISHNA MOHAN G V, BABU A N (Chemistry Dep, Koneru Lakshmaiah Education Foundation, Vaddeswaram- 522 502, Email: drkrishnamohangv@kluniversity.in) : RP-HPLC estimation of bumetanide and its impurities in oral solid dosage form. Asian J Chem 2019, 31(10), 2215-21.

A novel and simultaneous stability indicating RP-HPLC method has been developed for quantitative analysis of bumetanide in fixed dose pharmaceutical formulations. Bumetanide and its degradation products are well separated by the Discovery C₁₈, 250 × 4.6 mm, 5 µm column as a stationary phase and (50:50 v/v) of 0.1 % o-phthalaldehyde and acetonitrile as a mobile phase. All the compounds are monitored using photodiode array detector at 254 nm with an isocratic method and the flow rate of 1.0 mL/min was maintained. Validation of method was performed as per International Council for Harmonization (ICH) guidelines and the parameters namely; precision, accuracy, specificity, stability, robustness, linearity, limit of quantitation (LOQ) and limit of detection (LOD) were evaluated. The linearity of the proposed method was found to be 0.315-1.875 µg/mL for bumetanide and its impurities. The developed method is more economical and suitable for laboratory use because of solvent consumption is very less. Hence, the developed method can be used for the determination of bumetanide and its impurities in drug product stability studies and pharmaceutical formulations.

7 illus, 5 tables, 19 ref

005175   KUMAR D, SARASWATI (Chemistry Dep, Dr. Bhimrao Ambedkar Univ, Agra- 282 002, Email: devendrakumar131@gmail.com) : One pot microwave induced synthesis, characterization and antibacterial activity of tetrazamacrocyclic complexes of transition metal ions of bio-inorganic relevance. Asian J Chem 2019, 31(10), 2211-4.

Two new series of metal complexes, [M(C₁₈H₁₆N₄O₄)·2H₂O] (CH₃COO− )₂ and [M(C₂₂H₂₄N₄)·2H₂O] (CH₃COO− )2, where M= Co₂+/Ni₂+/ Cu₂+ have been prepared under microwave irradiation condition using microwave synthesizer. All the synthesized compounds were characterized by melting point determination of recrystallized samples, running single spot on TLC, elemental analyses, IR, UV-visible spectral studies. Synthesized macrocyclic complexes have been tested for their antibacterial activity against two bacteria Klebsiella pneumoniae and Escherichia coli by adopting disk diffusion method. The antibacterial activity was compared with amikacin antibiotic and it has been found that the complexes exhibited potential antibacterial activity. From the antibacterial studies, it has been found that the copper complexes were more effective on the microorganism in comparison to Ni(II) and Co(II) complexes.

1 illus, 2 tables, 33 ref

005221   ZAIDI S, CHATURVEDI D, SAXENA M, SRIVASTAVA R (Applied Chemistry Dep, Amity Univ, Lucknow- 226 028, Email: sadaf.zaidi00@gmail.com) : Synthesis and antimicrobial activity of dithiocarbamates of ω-substituted (2-naphthyloxy)alkanes. Asian J Chem 2019, 31(10), 2201-10.

A series of dithiocarbamates of ω-substituted (2-naphthyloxy) alkanes was developed through condensation of 2-(2-chloro-alkoxy)- naphthalene to various kinds of aliphatic, aromatic, alicyclic, heterocyclic primary and secondary amines employing benzyl trimethyl ammonium hydroxide in catalytic quantity (Triton-B/CS2 system) afforded desired products in high yields (82-98 %). The complete series of synthesized compounds (4-48) were evaluated for antimicrobial activity through microdilution method using various bacterial and fungal strains. The antifungal and antibacterial values were estimated as MIC values. Fluconazole and ciprofloxacin [16 to 0.03 µg/ mL] were used as the standard antifungal and antibacterial drug, respectively. Out of series of evaluated compounds, some of these compounds such as compounds 28, 29, 30, 31, 32, 33 have displayed maximum potency which is comparable to standard drugs.

2 tables, 48 ref

005216   SRIWAHYUNI E, PRODJOSANTOSO A K, SASMITA D (Chemistry Dep, Yogyakarta State Univ, Yogyakarta, Indonesia, Email: elsasriwahyuni.2017@student.uny.ac.id) : Zinc oxide supported onto biogenic silica from Gigantochloa atroviolacea leaves: Preparation, characterization and antibacterial activity. Asian J Chem 2019, 31(10), 2197-200.

Bamboo rod is a well known raw material utilized to make houses, papers, handicrafts, chopsticks and medicines. On the other hand, the utilzation of leaves, which are often considered as garbages, receive less attentions. Even though, bamboo leaves are good sources of SiO₂ or silica. This work reports the preparation of zinc oxide (ZnO) supported onto biogenic silica (SiO₂) from leaves of Gigantochloa atroviolacea, characterization and the antibacterial activities of ZnO@SiO₂ against Staphylococcus epidermidis. The ZnO was supported onto biogenic SiO₂ by using impregnation method of SiO₂ in zinc salt [Zn(NO₃)₂·6H₂O] solution. A combination XRD and SEM-EDX techniques were used to confirm the formation of ZnO on ZnO@SiO₂. Investigations indicate that the as prepared ZnO@SiO₂ revealed significant antibacterial activity against Staphylococcus epidermidis bacterial strain.

4 illus, 1 table, 40 ref

005204   RATHINAMANIVANNAN S, MEGHA K, CHINNAMANAYAKAR R, KUMAR A, EZHILARAS M R (Chemistry Dep, Prist Univ, Thanjavur- 613 403, Email: mrezhilarasi@gmail.com) : Synthesis and characterization of 2-pyrazoline derivatives and their in silico and in vitro studies on antimicrobial and anticancer activities. Asian J Chem 2019, 31(10), 2191-6.

The new series of 1-(4,5-dihydro-5-phenyl-3-diphenylpyrazol-1-yl)butan-1-one derivatives were synthesized by cyclization method using biphenyl chalcone with n-butyric acid and hydrazine hydrate. The synthesized 1-(4,5-dihydro-5-phenyl-3-diphenylpyrazol-1-yl)butan-1- one derivatives chemical structures were confirmed from spectral data such as FT-IR, 1 H and ¹³C NMR. 2-Pyrazoline derivatives were docked with bacterial (1UAG) and breast cancer (1OQA) protein. Based on high binding affinity score, the best compound was subjected to in vitro anticancer activity by MTT assay. Also, antimicrobial activity were studied for synthesized 2-pyrazoline derivatives.

2 illus, 2 tables, 13 ref

005213   SIVASANKARI G, SIVASANKARI K, NALINI T, PADMAPRIYA P, NADHIYA M (Chemistry Dep, Cauvery Coll for Women, Thiruchirappalli- 620 018, Email: sivakspm@gmail.com) : Selective determination of dopamine in presence of ascorbic acid using nafion coated methylene blue functionalized graphite electrode. Asian J Chem 2019, 31(10), 2185-90.

An electrochemical sensor has been developed using methylene blue (MB) functionalized graphite for the selective determination of dopamine in the presence of ascorbic acid. The immobilization of methylene blue on graphite was done by carbodiimide coupling method. The methylene blue functionalized graphite was characterized by SEM, FTIR spectroscopy and UV-visible spectroscopy. The immobilization of methylene blue functionalized graphite (MB-G) on the electrode surface was made by drop casting a small volume of MB-G dispersed methanol solution on the electrode surface. About 5 L of 0.5 % Nafion solution was also dropcasted for the stability and selectivity. The MB-G modified electrode was characterized by cyclic voltammetry. The modified electrode promotes the electrocatalytic oxidation of dopamine at a lower potential of 160 mV. The selective determination of dopamine in the presence of 100 times higher concentration of ascorbic acid was achieved by differential pulse voltammetry. The modified electrode offered a simple, selective and sensitive determination of low levels of dopamine. Also the oxidation over potential was reduced to an extent of 360 mV comparing with the bare graphite electrode. The proposed sensor has the advantage of easy fabrication, low cost, good sensitivity, reproducibility and stability.

9 illus, 30 ref