ALHARTHI A I
005145 ALHARTHI A I (Chemistry Dep, Prince Sattam Bin Abdulaziz Univ, Al-Kharj-11942, Email: a.alharthi@psau.edu.sa) : Simple protocol for the knoevenagel condensation under solvent free conditions using tungstophosphoric acid as catalyst. Asian J Chem 2019, 31(10), 2181-4.
The effect of calcination on the performance of tungstophosphoric acid for the product of Knoevenagel condensation was investigated. Substituted aldehydes and dimedone has been used in the presence of calcined tungstophosphoric acid as a heterogeneous catalyst using grinding method at room temperature. The results of reactions revealed that calcined tungstophosphoric acid has superior catalytic activity comparing to non-calcined catalyst in terms of yield and reaction time. Maximum yield of model compound was achieved by using 10 mol % of calcined catalyst in a reaction time that does not exceed 10 min, whereas the yield at same amount of non-calcined catalyst was 86 % in a reaction time of 35 min.
5 illus, 2 tables, 17 ref
SIRIJA M R, BALA D, RAMACHANDRAN D
005212 SIRIJA M R, BALA D, RAMACHANDRAN D (Chemistry Dep, Acharya Nagarjuna Univ, Nagarjuna Nagar- 522 510, Email: dittakavirc@gmail.com) : Partial molar volumes and spectral studies on binary mixtures of p-chloroacetophenone with aniline and n-alkyl anilines. Asian J Chem 2019, 31(10), 2173-80.
Ultrasonic velocities (u), viscosities (η) and densities (ρ) were measured for the binary mixtures of p-chloroacetophenone with aniline, N-methylaniline and N,N-dimethylaniline over the whole range of composition at different temperatures (303.15 K to 318.15 K) and at atmospheric pressure 0.1 MPa. Excess molar volume (VE ), deviation in viscosity (∆η) and deviation in isentropic compressibility (∆ks) have been calculated and fitted to Redlich-Kister polynomial equation to obtain their coefficients and standard deviations. The analyzed viscosity data of binary liquid mixtures were used to test the Grunberg-Nissan, Katti-Chaudari and Hind semi-empirical equations. The FTIR spectral study supports the experimental data to explain the molecular interactions between unlike molecules. Partial molar volumes of binary mixtures were evaluated for better understanding of intermolecular interactions of the above binary mixtures.
4 illus, 6 tables, 53 ref
GHOSHIR U G, KANDE S R, MULEY G G, GAMBHIRE A B
005164 GHOSHIR U G, KANDE S R, MULEY G G, GAMBHIRE A B (Chemistry Dep, Shri Anand Coll, Pathardi - 414 102, Email: abg_chem@ymail.com) : Synthesis and characterization of co-doped fly ash catalyst for chalcone synthesis. Asian J Chem 2019, 31(10), 2165-72.
A series of solid base fly ash hybrid materials were synthesized by doping alkali, alkaline earth metals with nitrogen, separately using coprecipitation process, combined with surfactant incorporating method. The catalysts were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy and photoluminescence spectroscopy. Results revealed that the co-doped hybrid materials are highly stable with particle size in the range of 40-60 nm. The surface basicity of fly ash was upraised by increased hydroxyl content by doping with alkali, alkaline earth metals with nitrogen. The basicity of hybrid material was measured by liquid phase, solvent free, single step condensation of 4-chlorobenzaldehyde and acetophenone giving higher conversion rate and selectivity of desired product chalcone. This conversion showed that the fly ash based hybrid material has sufficient basic site, responsible for the catalytic activity.
6 illus, 5 tables, 38 ref
PRITHIVIRAJAN B, JAS M J S, MARIMUTHU G
005199 PRITHIVIRAJAN B, JAS M J S, MARIMUTHU G (Bharathiar Univ, Coimbatore- 641 046, Email: gmarimuuthu@gmail.com) : Synthesis, characterization and in vitro antimicrobial evaluation of chalconeimine derivatives as potential inhibitors against enzymes produced from Staphylococcus aureus: A computational approach. Asian J Chem 2019, 31(10), 2157-64.
(Z)-1-(Benzo[d][1,3]dioxol-5-yl)-3-(4-(difluoromethoxy)-3-hydroxyphenyl)prop-2-en-1-one hydrazone derivatives pronounced in this manuscript represents a new collection of antibacterial agents in addition to the DNA gyrase inhibitors. Efforts had been made to synthesize those chalcone-hydrazone derivatives (4a-e) in good yields. The literature survey confirms that nano-ZnO as heterogeneous catalyst has obtained big interest because of its ecofriendly nature and has been explored as a effective catalyst for several organic ameliorations. Subsequently, induced by way of these observations and in continuation to our interest in organic synthesis with using nanocatalyst. in vitro Antibacterial activity has been evaluated towards Gram-positive and Gram-negative bacterial strains for all compounds. So one can discover the affinity to bacterial proteins docking have a look at have been carried out for 5 synthesized derivatives, antibiotic drug and co-crystallized ligands with special mechanism of action DNA gyrase B and methylthioadenosine/S-adenosylhomocysteine nucleosidase (MTAN) the usage of AutoDock 4.
5 illus, 6 tables, 35 ref
LEKHA V, PUSHPALETHA P
005183 LEKHA V, PUSHPALETHA P (Chemistry Dep, K.M.M. Government Women’s Coll, Kannur- 670 004, Email: lekhavdksm@gmail.com) : Indoor photochemistry involving ozone in rural location of Kannur−A tropical site in India. Asian J Chem 2019, 31(10), 2152-6.
This study reports the indoor ozone (O3) pollution in the rural location of Kannur, a tropical site in India, during March 2018 and the influence of their most important determinants. Measurements of indoor O3, NO, NO2 and NOx were carried out in a residential building for a period of one week. Measurements were taken from the kitchen, as it had been identified as the most polluted spot. The background concentrations of O3, NO, NO2 and NOx were also monitored. Indoor O3 originates mainly from the outdoor environment and is also produced from indoor sources. The results show that there is a higher level of indoor O3 during cooking hours. The study indicated that cooking activities in the kitchen had a strong impact on the indoor O3 level. Ozone is an important gaseous pollutant which may lead to severe health problems such as decreased lung function and respiratory symptoms.
4 illus, 31 ref
KUMAR D, SHARMA S
005176 KUMAR D, SHARMA S (Chemistry Dep, Dr. Bhimrao Ambedkar Univ, Agra- 282 002, Email: devendrakumar131@gmail.com) : Monitoring of organochlorine pesticides residues in five fruits using gas liquid chromatography equipped with electron capture detector (GLC-ECD). Asian J Chem 2019, 31(10), 2143-46.
India is the largest producer of fruits as they are important part of their economy. But they are badly affected by insect-pest attack during harvesting. Farmers use a large amount of pesticides to protect them but due to their longer persistence they found in fruits in small quantities. This paper described an analytical methodology for the monitoring of 20 organochlorine pesticides in 5 fruits viz. pineapple (Ananas comosus), apple (Malus pumila), plum (Prunus domestica), papaya (Carica papaya) and mango (Mangifera indica) by using gas liquid chromatography equipped with electron capture detector (GLC-ECD). During the monitoring work it has been found that each fruit was contaminated with pesticides. Pineapple was found contaminated with β-BHC, δ-BHC, heptachlor epoxide, dieldrin, endrin and methoxychlor; apple was found contaminated γ-BHC, δ-BHC, heptachlor epoxide, dieldrin, endrin, endosulfan II and methoxychlor; plum and papaya were found contaminated with γ-BHC, β-BHC, δ-BHC, heptachlor epoxide, 4,4′-DDE, endrin, endosulfan sulfate and methoxychlor; mango was found contaminated with β-BHC, δ-BHC, 4,4′-DDE, endrin, endosulfan sulfate and methoxychlor. However, the detected concentration of pesticides was below the MRL values but their long term use can cause serious health problems.
6 illus, 2 tables, 27 ref
MAHATO N R, HANSDA K M, DAS A, BANERJEE J, MONDAL S, MAHATA N
005185 MAHATO N R, HANSDA K M, DAS A, BANERJEE J, MONDAL S, MAHATA N (Chemistry Dep, Sidho-Kanho-Birsha Univ, Purulia- 723 104, Email: nagendranath_mahata.chem@skbu.ac.in) : Synthesis of mesoporous carbon xerogel and activation by oxidative treatment. Asian J Chem 2019, 31(10), 2139-42.
Synthesis of carbon xerogel and modification of its surface by various oxidative treatments are explored. Organic gel was synthesized by following the conventional sol-gel approach using formaldehyde and resorcinol. The wet gel was dried under subcritical condition and then carbonized, leading to carbon xerogel. Subsequently, the carbon xerogel was subjected to surface activation by means of oxidative treatment with nitric acid, sulphuric acid as well as aerial oxidation. Surface acid/base properties of the carbon xerogel have been strongly altered by treatments with nitric acid as well as with sulphuric acid. On the other hand, total surface area and pore volume have been significantly modified by air activation.
3 illus, 3 tables, 14 ref
MEHAN N, PANDURANGAN A, UPADHYAY P K, ALAM M S, BHATT S, KUMAR M, SAINI V, RISHABH
005186 MEHAN N, PANDURANGAN A, UPADHYAY P K, ALAM M S, BHATT S, KUMAR M, SAINI V, RISHABH (Maharishi Markandeshwar (Deemed to be Univ), Ambala, Haryana, Email: manish_singh17@rediffmail.com) : Phytopharmacology of Ficus religiosa L. and its significance as nanoparticulate carrier. Ann Phytomed 2019, 8(2), 186-93.
India is renowned for the development of health science based on Ayurveda, Unani, Siddha and Homeopathy. Ficus religiosa L. is most popular species in these indigenous system of medicines. In F. religiosa, entire plant parts like flowers, leaf, fruit, root, bark, inner part of stem, seeds are used as bioactive ingredients. Recently, some pharmacological reports presented that medicinally active molecules which are important for future medication are obtained majorly from trees. These reports also established an explanation related to antidiabetic, anticancer, antiulcer, anticonvulsant, cell reinforcement, and wound recuperating properties of various parts of F. religiosa. Different parts of F. religiosa (roots, leaves, bark, fruit and seed) contains different types of active constituents which may help to treat various diseases. Extractions of F. religiosa in solvents (Ethanolic extraction, Water extraction, Methanolic extraction, etc.) are depend on the type of disease. Particulate frameworks like nanoparticles have been utilized as a physical way to deal with adjust and improve the pharmacokinetic and pharmacodynamics properties of different kinds of drug molecules. Nanoparticles are very small materials in the size range from 1 to 100 nm. Distinctive kind of nanomaterials are being created by utilizing copper, zinc, titanium, magnesium, gold, alginate and silver. Nanoparticles of F. religiosa improve the medicinal property on different diseases like malignant growth, arthritis and so on. In this manner, the main intention behind writing this article is to present an advanced study on phytochemistry, pharmacological properites and nanotechnology of F. religiosa.
5 tables, 78 ref
RAMAKRISHNA J, WALI A F, BAKHIT F E M, ELAWAD A O, AYAABDIN
005201 RAMAKRISHNA J, WALI A F, BAKHIT F E M, ELAWAD A O, AYAABDIN (Pharmaceutical Chemistry Dep, RAK Medical and Health Sciences Univ, Ras AlKhaimah, UAE, Email: farooq@rakmhsu.ac.ae) : In vitro antioxidant activity and quantitative elemental analysis of Adansonia digitata L. fruit using inductively coupled plasma optical emission spectroscopy. Ann Phytomed 2019, 8(2), 127-33.
Adansonia digitata L.(AD) belongs to the family Malvaceae and genus Adansonia, native to the African continent. Various parts of this tree are used for health benefits as well as for food supplements. The dried fruits of AD were taken for the present study. Preliminary phytochemical screening of the different extracts of the fruits showed the presence of various secondary metabolites such as tannins, terpenoids, alkaloids, cardiac glycosides, phenolics, saponins, flavonoids and steroids. Since the fruits are rich source of vitamin C, the antioxidant screening of ethyl acetate and methanol extract were done by three different meth ods. 2,2-diphenyl-1-picrylhydrazyl, hydrogen peroxide and 2,2'-azino-bis (3-ethylbenzothiazoline-6-sulphonic acid), radical scavenging assays showed excellent antioxidant activity for the fruit of AD. The elemental analysis of the fruits was done by using ICP-OES and the results revealed the presence of various macronutrients (calcium, potassium, magnesium, phosphorus) and micronutrients (iron, sodium, manganese, zinc) in very good amount. The present study reveals that AD fruit can be used as a good source of antioxidant and in mineral deficiency ailments.
3 illus, 2 tables, 41 ref
VIJAYALINGAM T A, RAJESH N V
005220 VIJAYALINGAM T A, RAJESH N V (Tamil Nadu Veterinary and Animal Sciences Univ, Chennai- 600 051, Tamil Nadu, Email: tavijayalingam@gmail.com) : Seagrasses as potential source of fodder for livestock: Complete proximate and gas chromatography-mass spectrometry (GC-MS) analysis. Ann Phytomed 2019, 8(2), 93-8.
The present study analysed the nutritional values of Cymodocea serrulata (R.Br.) Asch. & Magnus, Syringodium isoetifolium (Asch.) Dandy and Enhalus acoroides (L.f.) Royle by complete proximate analysis and determined the phytocompounds present in them by using Gas Chromatography-Mass Spectrometry (GC-MS) technique. The complete proximate analysis revealed a higher content of crude protein, crude fibre, calcium, phosphorus and energy in all the three grasses under study. However E. acoroides contained higher content of ether extract, lower level of acid insoluble ash and gross energy compared to the other two grasses. The GC-MS analysis showed the presence of decane, sucrose, tetradecanoic acid, deoxyspergualin, n-hexadecanoic acid, phytol, ricinoleic acid, docosyl isobutyl ether and squalene in C. serrulata and decane, sucrose, phytol, 9,12,15-octadecatrienoic acid, (Z,Z,Z)-Triethylene glycol monododecyl ether and Hexadecanoic acid and 2-hydroxy-1-(hydroxymethyl) ethyl ester in S. isoetifolium. Ethanol extract of E. acoroides revealed the existence of decane, epoxomicin, tetradecanoic acid, n-hexadecanoic acid, phytol, linoelaidic acid, 9,12,15-octadecatrienoic acid, (Z,Z,Z)-diethylene glycol monododecyl ether, hexadecanoic acid, 1-(hydroxymethyl)-1,2-ethanediyl ester and 15,17,19,21-hexatriacontatetrayne in GC-MS study. All the three seagrasses under study were found to be the rich sources of crude protein, energy, minerals and phytocompounds of varied pharmacological properties which can enable them to be an eligible source of alternative nutritional supplements for ruminants in the areas adjacent to coastal region of Ramanathapuram district, where fodder scarcity exists.
3 illus, 4 tables, 26 ref
KHAN M S, DAS K
005173 KHAN M S, DAS K (Pharmacognosy and Phytochemistry Dep, Krupanidhi Coll of Pharmacy, Bangalore- 560 035, Karnataka, Email: drkkdsd@gmail.com) : Effect of solvents and extractors on proximate analysis, pharmacognostical screening and chromatographic analysis of Decalepis nervosa (Wight & Arn.) Venter leaf : An endangered plant from Western Ghats region. Ann Phytomed 2019, 8(2), 64-74.
Decalepis nervosa (DN) (Family: Apocynaceae), an endangered demanding medicinal plant of traditional system of medicine. The plant has been focused by many scientists for research and drug discovery sector. Its roots are used by tribal Indian for use as pickles. But still no research related to its medicinal as well as therapeutic values has been done. In the present study, leaf of the plant was evaluated for proximate analysis in terms of moisture content, ash values and extractive values. Histological nature of leaf was detected with powder microscopy and confirmed with scanning electron microscopy (SEM) of the plant for the first time. Further, leaf sample was extracted with 80 % methanol and aqueous solvents by conventional (soxhlet) and modern (microwave) extractors, followed by detail pharmacognostical screening through various chemical tests. Based on strong positive tests, contents of total phenolics and flavonoids were estimated. Thereafter, TLC and HPLC methods were applied for detection and analysis of particular secondary metabolites in both the extracts. Leaf powder microscopy as well as SEM study of leaf revealed the presence of epidermal cells, paracytic stomata, xylems, prismatic calcium oxalate crystals, unicellular covering trichomes, etc. Thereafter, estimated plant constituent resulted in high content of phenolics and flavonoids in microwave extracted methanolic extract (80 %). TLC and HPTLC study revealed the presence of gallic acid, rutin and quercetin and their content was high in 80 % methanolic extract (microwave method) than soxhlet method. Significant correlation was observed (p<0.001) among methanolic yield with the content of plant constituents. Pharmacognostical study, proximate analysis and extrac tion parameters of DN leaf identified the presence of phenolic compounds which helps in many therapeutic efficacies as well drug discovery in future.
9 illus, 7 tables, 30 ref
MEHROTRA N, JADHAV K, RAWALGAONKAR S, KHAN S A, PAREKH B
005187 MEHROTRA N, JADHAV K, RAWALGAONKAR S, KHAN S A, PAREKH B (Biochemistry Dep, Chauhan Institute of Science & Amrutben Jivanlal Coll, Mumbai- 400 056, Maharashtra, Email: nupur.mehrotra@mithibai.ac.in) : In vitro evaluation of selected Indian spices for α-amylase and α-glucosidase inhibitory activities and their spice-drug interactions. Ann Phytomed 2019, 8(2), 43-54.
India is believed to be crowned as the diabetes capital of the world by 2030. Considering the same, the present study was undertaken to elucidate the antidiabetic potential of selected Indian spices, viz., Cinnamomum zeylanicum Blume, Cuminum cyminum L., Laurus nobilis L., Piper nigrum L. and Elettaria cardamomum (L.) Maton. Phytochemical constituents of the spices were qualitatively identified and enzyme inhibitory assays performed. The study used 50 % hydroacetone extracts of the above-mentioned five spices to evaluate in vitro α-amylase and α-glucosidase inhibitory activities. The IC50 for α-amylase inhibitory activity were 706.04 ± 0.07, 517.51 ± 0.09, 349.41 ± 0.12, 573.21 ± 0.08 and 376.18 ± 0.12 g/ml, while those for α-glucosidase inhibitory activity were 243.92 ± 0.13, 386.73 ± 0.11, 203.01 ± 0.15, 269.92 ± 0.14 and 182.85 ± 0.16 g/ml for C. zeylanicum, C. cyminum, L. nobilis, P. nigrum and E. cardamomum respectively. Statistical analysis suggests that the highest α-amylase inhibitory activity was exhibited by L. nobilis and E. cardamomum while the highest α-glucosidase inhibitory activity was observed for E. cardamomum. Diabetes is a disorder associated with many complications and diabetics generally consume spices as nutraceuticals along with their drug regime. Thus, the spice-drug interaction with two commonly used drugs, viz., Acarbose-an antidiabetic and Losartanan antihypertensive were also studied. The results suggest that spice-drug interactions significantly enhanced the inhibitory activities of α-amylase and α-glucosidase. The maximum increase in percent α-amylase inhibitory activity with Acarbose supplementation was observed in C. zeylanicum (74.52 %) with minimum for E. cardamomum (50.53 %) while in presence of Losartan, maximum and minimum enhancement were observed for C. cyminum (48.34 %) and C. zeylanicum (28.19 %), respectively. As for modulation of percent α-glucosidase inhibitory activity with Acarbose, C. cyminum (52.42 %) showed the highest enrichment while no change was observed in the case of P. nigrum, while with Losartan maximal enhancement was with C. zeylanicum (19.85 %) and minimum with C. cyminum (5.4 %). Such interactions are a double-edged sword having an advantage but can also result in fatal consequences. Thus, for developing functional food having antidiabetic properties, the study of such interactions becomes significant.
7 illus, 11 tables, 71 ref
ASHIYA, DEI L, HARISHA C R, SHUKLA V J, SIVANANDAN A
005148 ASHIYA, DEI L, HARISHA C R, SHUKLA V J, SIVANANDAN A (PTSR Dep, IPGT & RA, Jamnagar, Gujarat, Email: ashiya221289@gmail.com) : Comparative pharmacognostical and pharmaceutical evaluation of Khadirashtaka kwatha and Khadirashtaka ghanavati - An ayurvedic formulation. J Phytopharmacol 2019, 8(5), 275-8.
Khadirashtaka Kwatha is an ideal medicine for Twak vikaras mentioned in many books of Ayurveda. This formulation consists of eight herbal drugs. Both the finished products (Khadirashtaka Ghanavati and Khadirashtaka Kwatha) are subjected to pharmacognostical evaluation, physico- chemical analysis like hardness, weight variation, loss on drying, ash value, pH value, water soluble extract, alcohol soluble extract, High Performance thin layer chromatography (HPTLC) etc. Pharmacognostical study showed the presence of certain identifying characters of all of the eight ingredients in the formulation like cork cells of Khadira, Crystal fibers of Nimba, scleroids of Haritaki, Bibhitaki and Amalaki, pitted vessels of Patola, starch cells of Guduchi, multicellular trichome of Vasa etc. Preliminary physicochemical analysis of Khadirashtaka Kwatha showed that ash value- 8.15%, loss on drying -9.35%, water soluble extract- 14.16%, methanol extract-10.72% and HPTLC showed 12 spots in 254nm and 6 spot in 366nm. Present work was carried out to compare the finished products like Khadirashtaka Ghanavati and Khadirashtaka Kwatha in terms of its identity, quality and purity so as to standardize the better form. Pharmacognostical and Physico-chemical observations revealed the specific characters of all active constituents in the preparations.
4 tables, 11 ref
NANDAKUMAR A, ASHOK KUMAR B N, ANGADI R, GEETHESH R R, MOHAN V
005191 NANDAKUMAR A, ASHOK KUMAR B N, ANGADI R, GEETHESH R R, MOHAN V (Rasashastra and Bhaishajya Kalpana Dep, Sri Dharmasthala Manjunatheshwara Coll of Ayurveda & Hospital, Udupi- 574 118, Email: aparnanandakumar08@gmail.com) : A comparative study on the pharmaceutical preparation of Kalyanaka Ghrita and Ksheerakalyanaka Ghrita. J Phytopharmacol 2019, 8(5), 260-5.
Kalyanaka Ghrita is a commonly prescribed formulation in cases of diseases of psychiatric origin like Unmada, Apasmara etc. The reference of Kalyanaka Ghrita is available in Brihattrayees, Sharangadhara Samhita, Chakradatta, Sahasrayoga, Kashyapa Samhita etc. The reference of Ksheerakalyanaka is mentioned along with the reference of Kalyanaka Ghrita in Chakradatta and also in Sahasrayoga. The reference mentioned in Charaka Samhita for Kalyanaka Ghrita and in Chakradatta for Ksheerakalyanaka Ghrita is taken for current study. The only difference observed in the references of both the formulations is the addition of two parts of Jala and four parts of Ksheera as Drava Dravya in case of Ksheerakalyanaka Ghrita. In case of Kalyanaka Ghrita only Jala is taken as Drava dravya. It is aimed to throw light on the pharmaceutical preparation of Kalyanaka Ghrita and Ksheerakalyanaka Ghrita in order to understand the aspects related to preparation of medicated Ghrita when Dugdha is mentioned as a Drava dravya.
11 illus, 6 tables, 3 ref
AJAYI G O, AKINSANYA M A, AGBABIAKA A T, OYEBANJO K S, HUNGBO T D, OLAGUNJU J A
005143 AJAYI G O, AKINSANYA M A, AGBABIAKA A T, OYEBANJO K S, HUNGBO T D, OLAGUNJU J A (Medical Biochemistry Dep, Lagos State Univ, Lagos, Nigeria, Email: gabriel.ajayi@lasucom.edu.ng) : D-Limonene: A major bioactive constituent in Allium fistulosum identified by GC-MS analysis. J Phytopharmacol 2019, 8(5), 257-9.
This investigation was carried out to determine the bioactive components present in Allium fistulosum by gas chromatography-mass spectrometry (GC-MS) analysis. The GC-MS analysis of the aqueous extract of the plant identified D-Limonene, a cyclic monoterpene, as the most abundant bioactive compound in A. fistulosum with approximately 99% of the total yield. Minor bioactive constituents present in the plant as revealed by GC-MS analysis include dichloroacetic acid (0.48%), α-pinene (0.36%), 1-Buten-3-yne, 1- chloro-, (Z)- (0.14%) and thymol, TMS derivative (0.07%). D-Limonene has been known to be commonly present in citrus peels, however, it is the first time this compound will be identified by GC-MS analysis as the major bioactive compound in A. fistulosum.
3 illus, 2 tables, 20 ref
ADAM O A O, ABADI R S M, AYOUB S M H
005142 ADAM O A O, ABADI R S M, AYOUB S M H (Pharmacognosy Dep, Al-Neelain Univ, Khartoum, Sudan, Email: osmanadam51@yahoo.com) : The effect of extraction method and solvents on yield and antioxidant activity of certain Sudanese medicinal plant extracts. J Phytopharmacol 2019, 8(5), 248-52.
This study came with the objective to compare the effect of extraction method and solvents on yield and antioxidant activity of certain Sudanese medicinal plant extracts, used in traditional medicine for treating various illnesses. The effect of maceration and Soxhlet successive extraction with n-hexane, chloroform and methanol were investigated on the antioxidant activity of five Sudanese medicinal plants. The antioxidant activities were assessed via DPPH (2, 2-Di (4-tert-octylphenyl)-1-picryl-hydrazyl) free radical scavenging activity and Propyl Gallate as standard antioxidants. Maceration was more effective than successive Soxhlet extraction with the same solvents.
2 illus, 6 tables, 23 ref
JAGWANI S, JALALPURE S, DHAMECHA D, HUA G S, JADHAV K
005168 JAGWANI S, JALALPURE S, DHAMECHA D, HUA G S, JADHAV K (KLE Academy of Higher Education and Research, Belagavi- 590 010, Email: jalalpuresunil@rediffmail.com) : A stability indicating reversed phase HPLC method for estimation of trans-resveratrol in oral capsules and nanoliposomes. Anal Chem Lett 2019, 9(5), 711-26.
Trans-resveratrol, a naturally occurring lipophilic polyphenol present in various foods, is well known for its therapeutic use. Owing to their exciting therapeutic potential, we developed a simple and precise stability indicating reverse-phase high performance liquid chromatography (RP-HPLC) method as per International Conference on Harmonization guidelines for quantitative analysis of trans-resveratrol in a commercial nutraceutical product and in-house nanoliposomes formulation. The chromatographic separation was attained on Phenomenex Luna C18 column (150 x 4.6 mm, 5 μm) at 30 °C using UV detection at 306 nm. The optimized mobile phase consisted of acetonitrile/water (30:70, v/v) at the flowrate of 1.0 mL/min under isocratic mode of elution. The proposed method was found to be accurate, precise and linear with regression coefficient of 0.999 which could analyse the samples with as low as in nanograms with percent recovery in the acceptable range of 97.97 - 102.80 %. In addition, stress degradation study was also carried out wherein analyte peak was found to be well resolved. Hence, the present investigation confirmed that the developed method can be employed for the analysis of trans-resveratrol in different formulations, and also of huge benefit in careful selection of experimental conditions and its implication for storage and formulation development.
42 ref
DONGALA T, KATAKAM L N R, PALAKURTHI A K, KATARI N K
005158 DONGALA T, KATAKAM L N R, PALAKURTHI A K, KATARI N K (Aurex Laboratories LLC, New Jersey- 08520, USA, Email: thirupathi2009@gmail.com) : RP-HPLC stability indicating method development and validation of pseudoephedrine sulfate and related organic impurities in tablet dosage forms, robustness by QbD approach. Anal Chem Lett 2019, 9(5), 697-710.
Pseudoephedrine is used for the temporary relief of stuffy nose and sinus pain/pressure caused by infection such as the common cold and flu. Here we were reporting a simple and precise validated stability indicating RP-HPLC method for estimation of Pseudoephedrine Sulfate and its related compounds in solid oral dosage forms. The stability indicating nature of current method has been demonstrated by a forced degradation study. All process related impurities and degradation products from forced degradation samples were well resolved from each other. The chromatographic separation of impurities was achieved with a Hypersil phenyl column (25 cm x 4.6 mm i.d., particle size 5 μ) using buffer and acetonitrile in the ratio of 95:5 v/v respectively as the mobile phase. The buffer used in mobile phase contained 10 mM potassium dihydrogen phosphate and its pH was adjusted to 3.0 ±0.05 with diluted orthophosphoric acid. The flow rate of HPLC was 1.0 mL min−1 and the wavelength of UV detector at 210 nm. The method was shown a linear response over range of 0.125 μg mL−1 to 0.750 μg mL−1 PES and impurities. The correlation coefficient was more than 0.999. Performed the robustness by using design experiments.
25 ref
KUMAR R P, EVANS D A, BABU K V D
005179 KUMAR R P, EVANS D A, BABU K V D (Zoology Dep, Government Coll of Women, Thiruvananthapuram, Kerala, Email: pradeepnta2005@gmail.com) : Characterization of multipotent compounds from Adiantum latifolium leaves by liquid chromatography-electrospray-mass spectroscopy. Anal Chem Lett 2019, 9(5), 682-96.
Adiantum latifolium Lam., a common fern rich in phytochemicals has been used in traditional medicine. We already reported the larvicidal and antibacterial effects of ethyl acetate fraction of methanol extract of its leaves against the coconut pest Oryctes rhinoceros. Bioactivity guided isolation of compounds from methanol extract of leaves of A. latifolium done by TLC, HPTLC analysis and column chromatography. The structural characterization of the bioactive compounds was done by interpreting their mass spectrum given by HPLC-ESI-Q-TOF-MS and comparison with authentic data. Various classes of phytocompounds viz. terpenoids, phenanthrenoids, phenolics and diones have been identified or tentatively characterized from the bioactive fraction showing a synergistic action. It presents a rapid and proactive method for simultaneous assay of biopotencies and characterization of phytocompounds for the preparation of improved natural pharmaceuticals, antimicrobials or biopesticides.
39 ref
TAMMAM M H, ABO-TALIB N F
005217 TAMMAM M H, ABO-TALIB N F (NODCAR, Giza, Egypt, Email: tammam.marva@gmail.com) : Development and validation of a bioanalytical HPLC method for quantification of valsartan in human plasma and its application in pharmacokinetics studies. Anal Chem Lett 2019, 9(5), 672-81.
Simple, sensitive, accurate and validated bioanalytical liquid chromatographic procedure coupled with fluorescence detector for estimation of valsartan in presence of diclofenac as internal standard (IS) in plasma has been established. The extraction of valsartan and IS was achieved using methyl tertiary-butyl ether: ethyl acetate (2:8) mixture and the extracted samples were separated on Waters, Xterra- C18 (150 x 4.6 mm, 5 μm) column with 1.0 mL/min flow rate. The detection has been performed at excitation and emission λ at 255 nm and 374 nm, respectively. The elution of the analytes was achieved using acetonitrile: phosphate buffer containing 1 g/L sodium salt of 1-Hexane sulphonic acid with pH adjusted to 2.5 with orthophosphoric acid (52:48, v/v) as an eluting system. The standard curves were linear from 5.0-4000.0 ng/ mL. Method validation has been prepared as per FDA guidelines. Good extraction recoveries of 87.22 % and 99.33 % for valsartan and IS have been acquired, respectively. The achieved values of accuracy and precision were in the adequate range. The proposed procedure was conducted effectively for analysis of valsartan after a single oral administration of one tablet of Tareg tablets ® (80 mg valsartan) to six healthy volunteers.
26 ref
AZIZUDDIN, KIRAN, YASMEEN K
005150 AZIZUDDIN, KIRAN, YASMEEN K (Chemistry Dep, Federal Urdu Univ of Arts, Science and Technology, Karachi- 75300, Pakistan, Email: azizpobox1@yahoo.com) : Nutritional changes in Shahzadi chilli during maturity from green to red stages. Anal Chem Lett 2019, 9(5), 664-71.
Capsicum annuum L. (chilli) is an important dietary source and provides vitamins A and C. In this study, physico-chemical properties, antioxidant analysis and metals accumulation were determined at green and red stages of Shahzadi chilli. The results indicated that the maximum physical properties including length (5.33 cm), diameter (0.672 cm), volume (16.1 cm3) and weight (4.94 g) were observed at green stage. Red chilli showed maximum nutritional components such as TDS (0.220 g/L), ash content (12.9 %), TSS (1.56 °Brix), TSC (793 mg/100 g) and total carotenoids (231 ppm). pH analysis of soil and water samples showed alkalinity. In antioxidant analysis, red chilli revealed higher TPC (1130 mg/100 g) and TFC (758 mg/ 100 g) with significant antioxidant activity by using DPPH radical scavenging assay (55.3 % inhibition) and RPA (1080 mg/100 g). Heavy metals analysis was also performed on chilli and soil. Fe (0.175), Ni (0.618) and Zn (0.114 ppm) were observed in high extent at red stage whereas higher Fe accumulation (36.4 ppm) was noted in soil. The resulting values of metals were with in safe limits in soil and chilli samples.
19 ref
ELOUDDARI A, AMRANI A E, SANCHEZ J A C, BELLAHCEN T O, ZOUTEIN A, EDDINE J J
005160 ELOUDDARI A, AMRANI A E, SANCHEZ J A C, BELLAHCEN T O, ZOUTEIN A, EDDINE J J (Extraction et Etude Physico-Chimique des Molécules Organiques, B P- 5366, Morocco, Email: alemrani77@yahoo.fr) : Chemical composition and biological activities of the Cladanthus mixtus essential oil: A review. Anal Chem Lett 2019, 9(5), 649-63.
A literature-based prospection of Cladanthus mixtus essential oil composition was carried out. Essential oils from this species are widely used in fragrances, cosmetics, soaps, detergents and perfumery. A review of the scientific literature pertaining to constituents of C. mixtus essential oils, volatile fractions and biological activities is presented. The results from this work indicate that the essential oil yield and chemical composition seem to be strongly dependent of collections sites. As well, these results support that C. mixtus can be a suitable alternative source of commercial chamomile oil and bioactive extracts.
57 ref
ELNAGGAR M M, GAWAD D A, BELAL T S
005159 ELNAGGAR M M, GAWAD D A, BELAL T S (Pharmaceutical Ananlytical Chemistry Dep, Alexandria Univ, Alaxandria, Egypt, Email: tbelaleg@yahoo.com) : Green simple spectrophotometric methods for determination of kanamycin sulfate using eosin and vanillin reagents. Anal Chem Lett 2019, 9(5), 634-48.
Two green and simple spectrophotometric methods were developed for the determination of kanamycin sulfate (KNM) in its dosage forms. Method I is based on formation of a binary complex with eosin in citric phosphate buffer pH 3.5 and the product was measured at 548 nm. Method II depends on the reaction of KNM with vanillin in borate buffer pH 12 to produce a colored chromogen, which showed maximum absorbance at 404 nm. Different experimental variables influencing development and stability of the colored products were optimized. Validation of the developed procedures regarding linearity, ranges, precision, accuracy, robustness and limits of detection and quantification was performed. The absorbance-concentration plots were found linear over KNM ranges of 1-5 and 5-30 μg/mL for methods I and II respectively. The validated methods were successfully applied to the analysis of commercial suspension containing the drug. The main advantages of the proposed methods are being simple, inexpensive, green (done almost entirely in aqueous media) and with no requirement for laborious extraction procedures.
36 ref
RANE V P, AHIRRAO V K, PATIL K R, JADHAV R A, INGLE R G, MORE K B, YEOLE R D
005202 RANE V P, AHIRRAO V K, PATIL K R, JADHAV R A, INGLE R G, MORE K B, YEOLE R D (Wockhardt Research Centre, Aurangabad- 431 006, Email: vipulrane@wockhardt.com) : Enantiomeric separation and thermodynamic investigation of (R)-5-[1-(4-Nitrobenzylsulfonyloxy)-ethyl]-5-(pyridine-2-yl)- [1,3,4]-thiadiazole, a key intermediate of nafithromycin. Anal Chem Lett 2019, 9(5), 625-33.
A selective and precise chiral high performance liquid chromatography method for the separation of (R)-5-[1-(4-Nitrobenzylsulfonyloxy)-ethyl]-5-(pyridine-2-yl)-[1, 3, 4]-thiadiazole (RE) has been developed and validated. It is an intermediate of a novel antibiotic nafithromycin. Nafithromycin is a ketolide class antibiotic being developed to treat community acquired bacterial pneumonia. Enantiomeric separation was achieved on Chiralpak IA column using mobile phase consisting of n-hexane and ethanol in the ratio of (15:85; v/v) with the resolution of more than 3. Separation was achieved at flow rate of 1.0 mL min−1 and column temperature 30 °C. The eluent was monitored at 254 nm. The developed method was validated as per the guideline. The method was found to be selective, precise, accurate and linear. Limit of detection and limit of quantification of the undesired enantiomer (S)-5-[1-(4-Nitrobenzylsulfonyloxy)-ethyl]-5-(pyridine-2-yl)- [1, 3, 4]-thiadiazole (SE) was 0.11 and 0.35 μgmL−1 respectively. Recovery of the SE was found to be in the range of 104.52 % and 105.83 %. The impact of thermodynamic parameters on the chiral separation was evaluated.
19 ref
CHAUHAN P, ANNU, HALVE A K, JAIN R
005153 CHAUHAN P, ANNU, HALVE A K, JAIN R (Environmental Chemistry Dep, Jiwaji Univ, Gwalior- 474 011, Email: priyachauhan0129@gmail.com) : Quantification of phytoestrogen genistein at graphite gold nanoparticle modified glassy carbon sensor in solubilized system. Anal Chem Lett 2019, 9(5), 608-24.
A novel graphite/gold nanoparticle modified glassy carbon electrode (GrNfs/AuNPs/GCE) sensor has been developed for the sensitive quantification of phytoestrogen genistein in solubilized system. The influence of experimental parameters on analytical performance of the fabricated sensor was investigated. GrNfs/AuNPs/GCE sensor exhibits excellent electrocatalytic performance toward oxidation of genistein in Britton Robinson buffer at pH 3.0 in solubilized system of 0.1% Triton X-100. Under optimized conditions, square wave anodic peak current shows a linear response for genistein oxidation over a concentration range of 0.8 μgmL−1 to 4 μgmL−1 with a correlation coefficient (R2) of 0.9987. The detection limit (LOD) and quantification limit (LOQ) were found to be 0.018 μgmL−1 and 0.987 μgmL−1, respectively. The developed sensor shows great promise for simple, sensitive, quantitative screening and detection of genistein using voltammetric techniques.
45 ref
PALAKURTHI A K, DONGALA T
005193 PALAKURTHI A K, DONGALA T (Aurex Laboratories LLC, New Jersey- 08520, USA, Email: thirupathi2009@gmail.com) : HPLC-UV method development for the determination of EDTA in oxycodone HCL oral liquids with derivatization technique robustness by design of experiments approach. Anal Chem Lett 2019, 9(5), 594-607.
This study deals with a simple and precise analytical method development and validation of a comprehensive high performance liquid chromatography method for estimation of Edetate disodium (EDTA) in liquid formulations. The effective chromatographic separation of EDTA was achieved with a X Bridge C-8 column with isocratic elution of mobile phase composed of buffer, methanol and water (175:90:675 v/v/v). The buffer used in mobile phase contained 0.06 % of tetra butyl ammonium hydroxide and adjusted pH to 7.5 ± 0.05 with 86 % of ortho phosphoric acid. The HPLC instrument flow rate was 2.0 mL min−1 and UV-detector wavelength was set 259 nm for the quantification of EDTA. The column oven temperature was 45 °C. The derivatization of EDTA was carried out using 1 % copper acetate solution to form a UV active chromophore group. Proved the robustness of the method by using Design of Experiments study. The correlation coefficient for EDTA was >0.9998 and linearity range was found to be 25-75 μg mL−1. The mean recovery values were found to 98.3 (50 % level), 98.8 (100 % level) and 98.4 (150 % level). Further, specificity of the current method was proved by separating the placebo peaks. The proposed validated HPLC method was successfully applied for the determination of EDTA in Oxycodon HCl oral solutions.
29 ref
AMIN A S
005146 AMIN A S (Chemistry Dep, Benha Univ, Benha, Egypt, Email: asamin2005@hotmail.com) : Solid phase extraction using polymer-based C18 cartridge modified with 5-(2‘-methyl-4‘-hydroxyphenylazo)-6-hydroxypyrimidine-2,4-dione for spectrophotometric determination of Indium(iii) in water and real samples. Anal Chem Lett 2019, 9(5), 582-93.
A novel highly selective, sensitive, and rapid procedure to determine nano-gram amount of In(III) depended on the speed reaction of In(III) with 5-(2‘-methyl-4‘-hydroxyphenylazo)-6-hydroxypyrimidine-2,4-dione (MHH-PD) and the colored complex extracted using solid phase extraction (SPE) have been developed. The interaction of MHHPD with In(III) to form a molar ratio 3: 1 [MHHPD to In(III)] violet complex is investigated in the presence of 3.0 M of nitric acid solution and Triton X-100 medium. The formed complex was enriched by SPE using a polymer-based C18 cartridge. In the reverse direction, the retained complex is eluted from the cartridge at a flow rate of 5.0 mL min–1 with 0.5 mL of acetonitrile. The enrichment factor of 200 was achieved. The molar absorptivity of the formed complex is 8.81 x 108 L mol–1 cm–1 at 622 nm. Beer’s law is obeyed in the range of 2.5-95 ng mL–1, whereas the optimum concentration ranges obtained from Ringbom plot was 5.0-90 ng mL–1. The relative standard deviation (RSD) for ten replicates sample of 60 ng mL–1 level is 1.15 %. The detection and quantification limits, are 0.75 and 2.47 ng mL–1. The proposed procedure was successfully applied to determine In(III) in sea, river, tap and waste waters, soil and sediment samples with good results comparing to the GFAAS method.
59 ref
TAHGHIGHI A, PARHIZGAR A R, KARIMI S, IRANI M
004005 TAHGHIGHI A, PARHIZGAR A R, KARIMI S, IRANI M (Clinical Research Dep, Pasteur Institute of Iran, Tehran, Iran, Email: atahghighi2009@gmail.com) : Synthesis of novel amodiaquine analogs and evaluation of their in vitro and in vivo antimalarial activities. J Vector Borne Dis 2019, 56(3), 221-30.
Due to the rapid increase of drug resistance in Plasmodium parasites, there is a pressing need of developing new antiplasmodial drugs. In this study, new amodiaquine (AQ) analogs were synthesized, followed by an evaluation of their antiplasmodial activity. A new series of quinoline derivatives containing N-alkyl (piperazin-1-yl)methyl benzamidine moiety was synthesized by reacting 4-[(4-(7-chloroquinolin-4-yl)piperazin-1-yl)methyl]benzonitrile with appropriate primary amines. The synthesized compounds were investigated for inhibitory activity by inhibition test of heme detoxification (ITHD). Their antiplasmodial activity was then evaluated using the classical 4-day suppressive test (Peter’s test) against Plasmodium berghei-infected mice (ANKA strain). The results showed that the percentage of heme detoxification inhibition in the active compounds was 90 %. The most promising analogs, N-butyl-4-[(4-(7-chloroquinolin-4-yl)piperazin-1-yl)methyl]benzamidine (compound 1e), and 4-[(4-(7-chloroquinolin-4-yl)piperazin-1-yl)methyl)]-N-(4-methylpentan-2-yl)benzamidine (compound 1f) displayed 97.65 and 99.18 % suppressions at the doses of 75 and 50 mg/kg/day, respectively. Further, the mean survival time of the mice treated with these compounds was higher than that of the negative control group. The newly synthesized amodiaquine analogs presented sufficient antiplasmodial activity with excellent suppressions and high in vitro heme detoxification inhibition. Higher mean survival time of the mice treated with synthetic compounds further confirmed the in vivo antimalarial activity of these new AQ analogs. Therefore, these compounds have the potential to replace common drugs from 4-aminoquinoline class. However, further investigations such as pharmacokinetic evaluations, cytotoxicity, toxicity, and formulation seem to be necessary.
5 illus, 3 tables, 26 ref
KUMAR H, WADI I, DEVARAJI V, PILLAI C R, GHOSH S K
003981 KUMAR H, WADI I, DEVARAJI V, PILLAI C R, GHOSH S K (Chemistry Dep, Visvesvaraya National Institute of Technology, Nagpur, Maharashtra) : A novel quinoline-appended chalcone derivative as potential Plasmodium falciparum gametocytocide. J Vector Borne Dis 2019, 56(3), 189-99.
Malaria has remained a global health problem despite the effective control and treatment measures. In the backdrop of drug resistance, developing novel hybrid molecules targeting the sexual stages (gametocytes) of the human malaria parasite Plasmodium falciparum is of great significance. Recently, chalconebased polyphenols have generated a great interest in the malaria research community worldwide due to their ease of synthesis and significant biological activity. The primary objective of this study was to investigate the interaction of a newly synthesized quinoline-appended chalcone derivative (ADMQ) with gametocyte specific proteins, Pfg 27 and Pfs 25 and explore its in vitro gametocytocidal potential. The characterization of ligand-protein interactions at the atomistic level was done by a simulation strategy that combines molecular docking and molecular dynamics (MD) simulation in a coherent workflow. The X-ray crystal structure of Pfg 27 was retrieved from protein data bank and Pfs 25 was built using the Iterative Threading ASSembly Refinement (I-TASSER) server. The detailed interaction of both ADMQ and a known gametocytocidal agent, methylene blue (MB) (used as a positive control) with gametocyte proteins Pfg 27 and Pfs 25 was studied with a 50 ns explicit MD simulation. The ligand binding pose in terms of glide score, molecular mechanics-generalized born surface area (MM-GBSA) binding energies, protein-ligand root-mean-square-deviation (RMSD) and secondary structure elements (SSE) changes were analyzed accordingly. The direct effect of ADMQ on structural integrity of P. falciparum gametocytes was also examined using in vitro microscopy. The analogous Glide score and MM-GBSA free energy of binding indicated stable interactions for both ADMQ and MB harboured in the active site of targeted gametocyte proteins, Pfg 27 and Pfs 25, separately. Explicit MD simulation by Desmond software package indicated similar distinguishable conformational changes in the active site of target polypeptide chain due to the specific accommodation of ADMQ molecule. The simulation also manifested comparable mechanistic profile in terms of protein-ligand RMSD and changes in secondary structure elements (SSE). Further, ADMQ treatment was found to adversely affect the structural integrity of gametocytes, which resulted in appearance of vesicles protruding from the gametocytes.The consolidated in silico molecular modeling and in vitro study described herein may give an insight into the interaction patterns of quinoline-chalcone hybrids with critical gametocyte proteins in the mosquito. This study will possibly pave the way for further exploration of similar heterocyclic quinoline-chalcone hybrids to open up new avenues in drug candidate development against P. falciparum gametocytes.
11 illus, 1 table, 44 ref
SANTOSH S R, SAMPATH S, GUPTA A
003998 SANTOSH S R, SAMPATH S, GUPTA A (Aviation Pathology and Toxicology Dep, Institute of Aerospace Medicine, Bengaluru, Karnataka, Email: santhuvet4u@gmail.com) : Simultaneous analysis of eight benzodiazepines in blood and urine matrix by gas chromatography–mass spectrometry: Implications for air crash investigation. Indian J Aerospace Med 2019, 63(1), 2-7.
Benzodiazepines are the most commonly prescribed class of drugs in India and are capable of impairing the performance of an aviator in therapeutic to subtherapeutic levels. Detection of benzodiazepines, particularly in blood, is not easy, since the concentrations present, especially following prescribed medical use, can be very low. Several publications have addressed estimation of benzodiazepines in plasma or serum; however, few have attempted their detection in whole blood. Urine, although a better specimen, benzodiazepines due to their extensive metabolism, its metabolites are excreted in urine instead of the parent compounds. In our laboratory, a method was developed for simultaneous detection and quantification of eight benzodiazepines in whole blood and urine matrix by gas chromatography–mass spectrometry selective ion monitoring (SIM) method. Chromatographic separation was optimized and achieved for separation of all 8 compounds using Agilent DB-5MS column. Retention time, selectivity and sensitivity were achieved by measuring each analyte in SIM mode. The developed method was tested and validated on actual biological samples for lorazepam, temazepam, diazepam, clonazepam, and nitrazepam. A single method was developed for the detection and quantification of eight benzodiazepines in whole blood and urine matrix by GC–MS SIM method. The method was also tested on limited number of actual biological samples for the lorazepam, temazepam, diazepam, clonazepam, and nitrazepam.
2 illus, 1 table, 12 ref
SINGH M V
004003 SINGH M V (Chemistry Dep, Banasthali Vidyapith, Rajasthan- 304 022, Email: manvir25365@gmail.com) : Deformation of virgin HD-PE, PP and waste PP Plastics into green fuel via a Pyrolysis-catalytic using a NiCO3 catalyst. Indian Chem Eng 2019, 61(3), 254-68.
Liquid green fuel or petrochemicals from virgin polypropylene, high-density polyethylene and waste PP were produced via a pyrolysis-catalytic cracking. Recycling which is a capable way of PP and HD-PE changing into green fuel. Pyrolysis-catalytic cracking was conducted at the temperature range 23– 370 °C with a NiCO3 catalyst and it helps need of alternative fuel. Green fuel was analysed by triple quadrupole GC–MS–MS, FT-IR spectroscopy, Perkin-Elmer series-II CHNS/O 24000, ICP, TGA its result founding into five categories as paraffin, cyclic paraffin, alcohols, esters and acetates. Conversion rates of virgin PP, HD-PE and waste PP into liquid green fuels were 87 %, 89 %, 90 %, light gases 12.28 %, 10.45 %, 9.51 % and residues 0.72 %, 0.55 %, 0.49% recovered from overall production process.
11 illus, 6 tables, 43 ref
BERGHEUL S, LIMONES-MÉNDEZ M, GROSJEAN J, HEHN A, OLRY A, BERKANI A
003952 BERGHEUL S, LIMONES-MÉNDEZ M, GROSJEAN J, HEHN A, OLRY A, BERKANI A (Mostaganem Univ, Mostaganem- 27000, Email: alexandre.olry@univ-lorraine.fr) : Comparative study of the production of coumarins and furanocoumarins in three Ruteae species. Indian J Nat Prod Resour 2019, 10(2), 137-42.
Within specialized metabolites, coumarins and furanocoumarins represent a wide group of structurally diverse compounds and are specially produced in plants belonging to the Rutaceae family. Here we performed the furanocoumarin and coumarin-targeted chemical characterization of three Ruteae species collected from Algeria. Detection and quantification of 27 coumarins and furanocoumarins extracted from stems and leaves was carried out by UHPLC-MS. We highlighted significant chemical differences between these plants. Ruta chalepensis L. is the highest producer with 24.83 mmol/g dry material in stems and 15.70 mmol/g dry materials in leaves while Haplophyllum tuberculatum (Forsk.) is the lowest producer. We also showed a surprising chemical diversity between R. chalepensis L and R. angustifolia Pers. This chemical diversity might, therefore, be a helpful tool for phylogenetic identification of plants.
1 illus, 2 tables, 37 ref
TUKIRAN, WARDANA A P, HIDAJATI N, SHIMIZU K
004008 TUKIRAN, WARDANA A P, HIDAJATI N, SHIMIZU K (Chemistry Dep, Negeri Surabaya Univ, Surabaya, Indonesia, Email: tukiran@unesa.ac.id) : Chemical components and antioxidant activities of methanol extract of Syzygium polycephalum Miq. stem bark (Myrtaceae). Indian J Nat Prod Resour 2019, 10(2), 127-36.
This study aimed to reveal chemical components and screen antioxidant activity of methanolic extract of Syzygium polycephalum stem bark. The chemical components were isolated by using column chromatographic techniques and determined by spectroscopic methods (UV-Vis, FTIR, MS, and NMR) and comparison with literature data, in which the antioxidant activity was performed using 2,2’-diphenyl-1-picrylhydrazyl (DPPH). The present investigation resulted in four compounds involving gallic acid, pinostrobin, 3,4,3’-tri-O-methylellagic acid, and 3,3’-di-O-methylellagic acid. The four compounds were all in the form of phenolic compounds found from the extract whereas 3,4,3’-tri-O-methylellagic acid and 3,3’-di-O-methylellagic acid were ellagic acid derivatives. The methanolic extract, the four compounds, and vitamin C (as positive control) showed antioxidant activity against DPPH with the IC50 value of 99.9; 10.0; 183.2; 72.1; 63.3; and 13.9 µg/mL, respectively. The antioxidant activity of gallic acid was more active than that of vitamin C. The present study confirms that Syzygium polycephalumis rich in phenolic compounds and natural antioxidants.
4 illus, 5 tables, 42 ref
BAGHEL A, BHUVANESWARI A, SINGH V V, BOOPATHI M, SINGH B
003948 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 characterisation 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 (68 m2/g) was found to be more than that of NIP (24.6 m2/g) and CdP (17 m2/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
DUTTA M, DUTTA P
003964 DUTTA M, DUTTA P (Chemistry Dep, Bejoy Narayan Mahavidyalaya, Itachuna - 712 147, Hooghly, Email: pimidu@yahoo.com) : Investigation of fatty acid content in the edible portion of long-whiskered catfish Sperata aor. Biosci Biotech Res Asia 2019, 16(3), 577-80.
The composition of fatty acid of Sperata aor, a fish consumed as food by the people of gangetic West Bengal, India was investigated to determine its nutritional value. Our investigation shows the presence of PUFA’s namely EPA (0.22%), DHA (0.74%), Linolenic acid (0.39%), Linolelaedic acid (30.45%), ã-Linolenic acid (0.24%), Eicosatrienoic acid (0.38%), Arachidonic acid (0.55%) in the fish. The biosynthetic pathway for the synthesis of prostaglandins and cell membranes in mammals requires the presence of Linolelaidic acid which is present in good quantity in this fish. However, its high concentration in human body may lead to heart ailments also. Arachidonic acid, associated with growth, development and health of infants as well as adults is present in the fish. Palmitoleic acid (C16:1) a constituent of adipose tissue in humans, is also present in the fish (42.29%), has the ability to suppress inflammation, and is also known to combat obesity. Though presence of low total SFA (6.20%) is positive nutritional aspect the consumption of this fish however should be restricted due to its not so healthy ù-3:ù-6 ratio (1:4).
1 table, 21 ref
RAMPRIYA S, KUMAR N S
003993 RAMPRIYA S, KUMAR N S (Chemistry and Bioprospecting Div, Institute of Forest Genetics and Tree Breeding, Coimbatore, Tamil Nadu, Email: senthilnk@icfre.org) : Characterization of anthocyanins from red tamarind, Tamarindus indica var. rhodocarpa using spectral analysis. Int J Pharm Biol Sci 2019, 9(3), 926-31.
To characterize anthocyanin from Tamarindus indica var rhodocarpa using spectral analysis for use in food colourants. Nutritional parameters such as carbohydrate and protein contents were high in Red Tamarind unripen fruit extract with the values of 8.6 g and 12.61 g respectively. Low fat level with nil Cholesterol (BDL) is present in the extract. Other minerals and vitamins such as iron, calcium, vitamins A &C are rich in the extract. TLC separation of unripen fruit extract of red tamarind matched with the authentic anthocyanins pigments namely, cyaniding-3-glucoside, delphidin and pelargonidin. HPLC analysis also confirmed the presence of major anthocyanin pigments, cyaniding-3-glucoside, delphidin and pelargonidin. Anthocyanins are the important polyphenolic compounds present in Red Tamarind. The characterization of anthocyanins using TLC and HPLC analysis revealed the presence of three major anthocyanins pigments v: z., cyanidin-3-glucoside, pelargonidin, delphinidin. The red colour of the unripen fruit extracts of red tamarind is due to presence of cyaniding-3-glucoside with higher quantity of 94.21%. The pH of the extract is 2. Analysis of nutritional parameters revealed that the extract contains high level of protein and carbohydrate; rich in minerals and vitamins with low level of fat which support the daily human intake values, hence it may be considered to use as food colourant. Therefore, it is concluded that the presence of anthocyanin pigments cyaniding-3-glucoside in unripen fruit of red tamarind is responsible for red colour which is depending on the pH.
4 illus, 2 tables, 23 ref
DAMLE M C, PARDESHI K K
003959 DAMLE M C, PARDESHI K K (All India Shri Shivaji Memorial Society’s Coll of Pharmacy, Pune- 411 001, Email: mcdamle@rediffmail.com) : Stability indicating chromatographic method for estimation of methimazole. Int J Pharm Biol Sci 2019, 9(3), 843-58.
A stability indicating high performance thin layer chromatography (HPTLC) method was developed and validated for determination of anti-thyroid drug, Methimazole. HPTLC separation was carried out on Merck TLC aluminium sheets precoated with silica gel 60F 254 using mobile phase as Chloroform: Acetone. Methimazole gave sharp peak at Rf 0.44 ± 0.03 at 252 nm. Calibration curve was linear in range 200-600 ng/band for methimazole. Stress degradation study was carried out according to ICH guidelines Q1A (R2) and the method was validated as per ICH guideline.
5 illus, 5 tables, 12 ref
RAGHAVENDRA N, HUBLIKAR L V, PATIL S M, GANIGER P J, BHINGE A S, CHITNIS S
003992 RAGHAVENDRA N, HUBLIKAR L V, PATIL S M, GANIGER P J, BHINGE A S, CHITNIS S (Chemistry Dep, K.L.E. Society's P. C. Jabin Science Coll, Hubballi- 580 031, Email: rcbhat3@gmail.com) : Corrosion protection of expired perindopril and expired alprazolam drug in carbon steel in the 3 % NaCl solution. Int J Pharm Biol Sci 2019, 9(3), 838-42.
Present study aimed at the application of expired Perindopril and Alprazolam drug as a corrosion inhibitor for the carbon steel in the 3 % NaCl solution. Two techniques (weight loss and atomic absorption spectroscopy) used to evaluate the corrosion inhibition mechanism. Weight loss technique revealed that, the corrosion inhibition property of expired Perindopril and expired Alprazolam drug is mainly depends upon the concentration of the expired species and solution temperature. The atomic absorption spectroscopy (AAS) technique fully supports the results of weight loss studies. Among the expired Perindopril and Alprazolam drug species, expired Perindopril drug exhibit the superior corrosion inhibition property on the carbon steel in the 3 % NaCl solution.
2 illus, 2 tables, 10 ref
BHALERAO R A, MEHTA D R, RAKA N K, MARKAD A M, PAWAR A R, UNDRE P S, DAMLE M C
003954 BHALERAO R A, MEHTA D R, RAKA N K, MARKAD A M, PAWAR A R, UNDRE P S, DAMLE M C (All India ShriShivaji Memorial Society’s Coll of Pharmacy, Pune- 411 001, Email: mcdamle@rediffmail.com) : Stability indicating HPTLC method for hesperidin. Int J Pharm Biol Sci 2019, 9(3), 832-7.
A stability indicating assay method was developed and validated according to the ICH guidelines for estimation of Hesperidin using HPTLC. Hesperidin is flavonoid with anti-inflammatory, anti-oxidant properties. The objective was stability-indicating method development and validation for Hesperidin by HPTLC. HPTLC method was developed and validated using Mobile phase consisting of Ethyl acetate: Methanol: Water (7:2:2 v/v/v) and detected at wavelength 283 nm. Various forced degradation conditions were used to check degradation of drug. The method showed a good linear relationship (r 2= 0.9855) in the concentration range 200-1000 ng/band. It was found to be linear, accurate, precise and specific. The proposed HPTLC method for Hesperidin can be applied for quality control as well as for stability testing of Hesperidin. The developed method was validated as per ICH guideline Q2(R1).
4 illus, 5 tables, 13 ref
BAROT A A, PANCHAL T M, PATEL A, PATEL C M, SINHA V K
003950 BAROT A A, PANCHAL T M, PATEL A, PATEL C M, SINHA V K (Byblos Roads Marking and Traffic Signs LLC, United Arab Emirates, Email: amit_ic@outlook.com) : Polyester the workhorse of polymers: A review from synthesis to recycling. Arch Appl Sci Res 2019, 11(2), 1-19.
In this age of polymer, polyester still conquered the leading position amongst the other manmade polymers. Polyester has become the focus of interdisciplinary research and received considerable attention due to their unique chemical and physical properties as well as their potential applications. Also, we accomplished from the recent researches that polyester is involved either in one or the other form in many works. Thus we show our deliberation to make a platform for those researchers who show interest in work on polyesters, where they find enough basics related to polyesters and its current scenario. In this framework, this review provides the extractive information’s about the polyesters, which covers from to its development, chemistry, application fields up to the methods of recycling used in present scenario.
5 illus, 4 tables, 170 ref
HAZRA G, MITRA P, DAS T
003971 HAZRA G, MITRA P, DAS T (Chemistry Dep, Burdwan Univ, Burdwan– 713 104, Email: tdas.bu@gmail.com) : Preparation and properties of lead-iron-phosphate nuclear waste glasses. Trans Indian Ceram Soc 2019, 78(2), 69-77.
Lead-iron phosphate (LIP) glasses are a promising new waste form for safe immobilization of both high level defence and high level commercial radioactive waste for long term disposal. LIP glasses have several advantages such as lower aqueous corrosion rate, lower processing temperature, etc. The durability test for LIP glasses showed that the alkaline earth oxides BaO, SrO and CaO decrease the durability while PbO, Fe2O3 and CeO2 improves the corrosion resistance. For some LIP glass samples containing uranium the leach rates as calculated from BET surface areas were in the range of 8.210–4 to 4.310–3 g.m–2.h–1 at 90 oC which is 1000 times lower than that of the borosilicate glasses. Thermal study shows that the glass transition temperature was in the range of 360o -400 oC for the LIP glasses. IR studies show absorptions at 520, 1025, 1700, 2225 and 3450 cm–1. The observed IR and Raman scattering spectra are representative of a mixture of chain terminating Q1 species and chain forming Q2 species. From the radiotracer leaching studies the role of Ce4+ as good binder-modifier is established. The values of isomer shift in the Mössbauer spectra increases with increasing Fe2O3 content.
12 illus, 3 tables, 49 ref
DAS D, KAYA N
003960 DAS D, KAYA N (CSIR- Central Glass and Ceramic Research Institute, Kolkata– 700 032, Email: nijhuma@cgcri.res.in) : Thermal shock resistance of porous silicon carbide ceramics prepared using clay and alumina as additives. Trans Indian Ceram Soc 2019, 78(3), 165-71.
Porous silicon carbide ceramics were prepared by an in situ reaction bonding process using clay and alumina as additives. The effects of alumina additive, pore former on phase composition, microstructure, flexural strength and thermal shock resistance of the ceramics were studied. Thermal shock resistance of porous SiC ceramics due to cooling was evaluated as a function of quenching temperatures and quenching cycles using water- and air-quenching technique. It was observed that residual strength of the quenched samples in water decreased with increase in the quenching temperature but was almost independent of quenching cycles. In water quenching, the surface of the sample cooled almost instantly but the inside remained hot which created an uneven thermal profile and generated microcracks in the sample; as a result sudden reduction of flexural strength was observed. The results showed that flexural strength and thermal shock resistance properties of the ceramics prepared with alumina are better than those of the ceramics prepared without alumina and the material was found suitable for hot gas filtration application.
12 illus, 1 table, 26 ref
BHATTACHERJEE A K, SHUKLA P K, DIKSHIT A
003955 BHATTACHERJEE A K, SHUKLA P K, DIKSHIT A (ICAR–Central Institute for Subtropical Horticulture, Lucknow- 226 101, Email: bhatchaj_ak@yahoo.com) : Dissipation of imidacloprid residues in mango orchard soil quantified by HPLC. J Eco-friendly Agric 2019, 14(2), 50-3.
Imidacloprid, a neonicotinoid insecticide, is widely used in mango ecosystem to control mango hopper at prebloom stage. Persistence of imidacloprid in soil is well reported. While spraying any insecticide to a tree, some portion does come in contact with rhizosphere soil. Hence after spraying at 0.005 per cent to mango (cv. Dashehari) trees, its residue was analyzed in rhizosphere soil by HPLC. Soil samples were extracted with acetonitrile by vortexing followed by ultrasonic solvent extraction without any cleanup. Imidacloprid dissipated from its initial deposit of 0.760 mg g-1 at zero day to 0.044 mg g-1 after 60 days of spraying in mango orchard soil (Sandy loam). After 60 days of application, 94.21 per cent of imidacloprid degradation was recorded in soil. The dissipation rate followed pseudo first-order kinetics in soil with calculated half-life (DT50) value of 17.5 days. Imidacloprid has been found a persistent insecticide in mango orchard soil.
1 illus, 3 tables, 23 ref
BORA G, GOGOI D, SAIKIA S, PAREEK A, HANDIQUE J G
003956 BORA G, GOGOI D, SAIKIA S, PAREEK A, HANDIQUE J G (Chemistry Dep, Dibrugarh Univ, Dibrugarh- 786 004) : Stannous chloride catalyzed synthesis of Schiff bases from hydroxybenzaldehydes and determination of their antioxidant activity by ABTS and DPPH assay. J Chem Sci 2019, 131(8), 68.
Phenolic compounds play a very important role in human life because of their antioxidant activity which can prevent harmful diseases caused by free radicals. In the present work, we have synthesized some Schiff bases by the reaction of different hydroxybenzaldehydes and primary aromatic diamines using Stannous Chloride (SnCl2⋅2H2O) as the catalyst. The products were characterized by FT-IR spectroscopy, GCMS and NMR spectroscopy. Furthermore, the antioxidant activity of the Schiff bases were determined by using DPPH assay and ABTS assay and the results were compared with a standard compound, trolox as well as with the parent aldehydes. The synthesized compounds were found to have better antioxidant activity than their corresponding parent aldehydes.
22 ref
FAISAL M, SAEED A, HUSSAIN S, DAR P, LARIK F A
003967 FAISAL M, SAEED A, HUSSAIN S, DAR P, LARIK F A (Chemistry Dep, Quaid-i-Azam Univ, Islamabad- 45320) : Recent developments in synthetic chemistry and biological activities of pyrazole derivatives. J Chem Sci 2019, 131(8), 70.
Pyrazole, a five-membered heterocycle containing two nitrogen atoms, is extensively found as a core framework in a huge library of heterocyclic compounds that envelops promising agro-chemical, fluorescent and biological potencies. Attributed to its several potential applications, there is a rise in the significance of designing novel pyrazoles, disclosing innovative routes for synthesizing pyrazoles, examining different potencies of pyrazoles, and seeking for potential applications of pyrazoles. This review consists of two parts. The first part provides an overview on the recent developments in synthetic approaches to pyrazoles, which is related to the new or advanced catalysts and other ‘environment-friendly’ procedures, including heterogeneous catalytic systems, ligand-free systems, ultrasound and microwave-assisted reactions. The second part focuses on the recently reported novel biological affinities of pyrazoles. This systematic review covers the published studies from 1990 to date. It is expected that this review will be helpful in future research and for new thoughts in the quest for rational designs for developing more promising pyrazoles.
126 ref
BANERJEE I, GHOSH K C, SINHA S
003949 BANERJEE I, GHOSH K C, SINHA S (Indian Association for the Cultivation of Science, Kolkata- 700 032) : Pd-catalyzed C–H bond activation of Indoles for Suzuki reaction. J Chem Sci 2019, 131(8), 71.
We present a practical method for Suzuki coupling by which unprotected or N-protected indoles may be selectively arylated in the C2-position through direct C–H bond activation by electrophilic Pd(TFA)2 catalyst. The protocol is operationally simple as it is carried out in dioxane/water mixture, and air as the sole oxidant at room temperature. Various 2-arylated indoles were obtained in good yields. The protocol works for benzofuran, pyrrole and thiophene also.
24 ref
SARAVANABHARATHI D, OBULICHETTY M, KUMARAVEL M
003999 SARAVANABHARATHI D, OBULICHETTY M, KUMARAVEL M (Chemistry Dep, PSG Coll of Technology, Coimbatore- 641 004) : Facile crystallization of 2-phenyl benzimidazole-5-sulfonic acid: Characterization of lattice water dependent zwitterionic supramolecular forms, with modulation in proton conductivities. J Chem Sci 2019, 131(8), 72.
A facile aqueous medium crystallization strategy has been found for this water insoluble title compound. Two crystalline forms, differing in the number of lattice water molecules (mono hydrated; form I & di-hydrated; form II), have been obtained, depending on the duration of crystallization. X-ray structural studies reveal that the compound crystallizes in the zwitterionic state in both the forms, due to the protonation of one imidazole nitrogen by –SO3H group, are engaged in hydrogen bonded interactions, involving lattice water molecule(s), and thus the supramolecular arrangements of the forms are influenced by lattice waters. Additional water molecules in the form II make it more hydrophilic, as confirmed using contact angle measurements. Procedures were optimized for better crystalline yields, and the bulk purity were ascertained by TGA, elemental and PXRD analysis. AC impedance measurements prove that both the crystalline forms are indeed proton conducting electrolytes, with magnitudes of 1×10−5 S cm−1 1×10−5 S cm−1 and 5×10−5 S cm−1 5×10−5 S cm−1 for form I & II, respectively under humidified conditions at 25 ∘C. Proton conducting performance of II has been found to be greater than I and could be correlated with its higher hydrophilicity and enriched hydrogen bonds for Grotthuss mechanism.
11 illus, 1 table, 48 ref
LIU Q, XIE B, SEN L, LIAO Q, DENG R, ZHAOHUA Y
003983 LIU Q, XIE B, SEN L, LIAO Q, DENG R, ZHAOHUA Y (Chemistry Dep, Nanchang Univ, Nanchang- 330 031) : Silicon-containing diorganotin complexes with salicylaldehyde thiosemicarbazone and their anticancer activity. J Chem Sci 2019, 131(8), 73.
Eight novel silicon-containing diorganotin complexes with salicylaldehyde thiosemicarbazone were synthesized. They were characterized by 1H NMR, 13C NMR, IR spectra, elemental analysis and X-ray single-crystal diffraction. Spectroscopic and X-rays studies indicated that the thiosemicarbazone Schiff base and tin atom were coordinated as a parallel five- and six-membered heterocyclic structure. In addition, the bioassay of the synthesized complexes was performed and the results show that the silicon-containing diorganotin complexes with salicylaldehyde thiosemicarbazone have good anticancer activity on human breast cancer cells.
2 illus, 4 tables, 22 ref
GOGOI N G, HANDIQUE J G
003969 GOGOI N G, HANDIQUE J G (Chemistry Dep, Dibrugarh Univ, Dibrugarh- 786 004) : Novel protocol for synthesis of 1,4-diiminocurcumin stabilized silver nanoparticles and application as heterogenous recyclable catalyst and antibacterial agent. J Chem Sci 2019, 131(8), 74.
Curcumin [(1E, 6E)-1,7-bis(4-hydroxy-3-methoxy-phenyl)-1,6-heptadiene-3,5-dione] is a low molecular weight yellow-orange polyphenolic pigment extracted from the powdered rhizome of Curcuma longa. Curcumin has wide medicinal applications as an antioxidant, anti-inflammatory, cancer chemopreventive, and potentially chemotherapeutic agents as well as stabilizer/reducing agent in silver nanoparticles (AgNPs) synthesis. However, the low solubility of curcumin in aqueous solutions limits its applications and also, many of AgNP synthetic processes lack a greener synthetic route. In the present work, a Schiff base of curcumin is synthesized condensing curcumin and 1,4-diaminobutane in 2:1 ratio. The resulting product shows improvement in solubility in water and favours the synthesis of AgNPs in aqueous medium at room temperature, acting as a self-reducing/stabilizing agent. This proposed synthetic route is simple, feasible and green. The size and morphology of AgNPs are analyzed by TEM, SEM, EDS and XRD techniques. The recyclable AgNPs as a heterogeneous catalyst in the reduction of nitroaromatics to amino compounds is environmentally benign and can be re-used up to 5th cycle without considerable loss of its catalytic activity. Moreover, both Cur-1,4 and AgNPs show bactericidal properties against bacterial strains (Bacillus subtilis, Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa) which find medicinal importance in future.
8 illus, 1 table, 52 ref
ZEROUAL A, RIOS-GUTIERREZ M, SALAH M, ABDALLAOUI H E A E, DOMINGO
004011 ZEROUAL A, RIOS-GUTIERREZ M, SALAH M, ABDALLAOUI H E A E, DOMINGO (Chouaïb Doukkali Univ, El Jadida- 24000) : An investigation of the molecular mechanism, chemoselectivity and regioselectivity of cycloaddition reaction between acetonitrile N-Oxide and 2,5-dimethyl-2H-[1,2,3]diazaphosphole: A MEDT study. J Chem Sci 2019, 131(8), 75.
The [3+2] cycloaddition (32CA) reactions of acetonitrile N-oxide with 2,5-dimethyl-2H-[1,2,3]diazaphosphole has been studied using the Molecular Electron Density Theory (MEDT) through DFT calculations at the B3LYP/6-31G(d,p) computational level. Analysis of the relative free energies associated with the competitive ortho and meta reaction paths shows high chemo- and regioselectivity for this 32CA reaction in clear agreement with the experimental outcomes. The topological analysis of the electron localization function (ELF) of the selected points of the IRC associated with the formation of the P-C and C-O single bonds indicates a zwitterionic type structure. The 32CA reaction takes place through a two-stage one-step mechanism initialized with the formation of the P-C single bond.
5 illus, 1 table, 32 ref