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- Author or Editor: G. Jain x
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Summary
A new, specific, sensitive, selective, precise, and reproducible high-performance thin-layer chromatographic (HPTLC) method has been established for study of the stability of 3-acetyl-11-keto-β-boswellic acid (AKBA). HPTLC was performed on aluminium foil plates coated with 200 μm silica gel 60F254. Linear ascending development with toluene-ethyl acetate 7:3 (v/v) was performed at room temperature (25 ± 2°C) in a twin-trough glass chamber saturated with mobile phase vapour. Compact bands (R F 0.52 ± 0.02) were obtained for AKBA. Spectrodensitometric scanning was performed in absorbance mode at 250 nm. Linear regression analysis of the calibration plots showed there was a good linear relationship (r 2 = 0.9989 ± 0.0002) between peak area and concentration in the range 200–1200 ng band−1. The method was validated for precision, recovery, robustness, specificity, and detection and quantification limits, in accordance with ICH guidelines. The limits of detection and quantification were 3.06 and 9.29 ng band−1, respectively. The recovery of the method was 99.35–100.21%. AKBA was subjected to various stress test conditions — acid and alkali hydrolysis, oxidation, photodegradation, and dry and wet heat treatment. Degradation products were well resolved from the pure drug with significantly different R F values. Statistical analysis showed the method could be successfully applied for the estimation of AKBA in herbal extract and in nanoparticles. Because the method could effectively separate the drug from its degradation products, it can be regarded as stability-indicating.
Summary
A simple, rapid, and specific reversed-phase HPLC method has been developed for simultaneous analysis of withaferin-A and 6-gingerol in a polyherbal formulation containing Withania somnifera and Zingiber officinalis extracts. HPLC analysis was performed on a C18 column using a 40:60 (v/v) mixture of acetonitrile and water as isocratic mobile phase at a flow rate of 1.5 mL min−1. UV detection was at 227 nm for withaferin-A and 278 nm for 6-gingerol. The method was validated for accuracy, precision, linearity, specificity, and sensitivity in accordance with International Conference on Harmonization guidelines. Validation revealed the method is specific, accurate, precise, reliable and reproducible. Good linear correlation coefficients (r 2 > 0.9996) were obtained for calibration plots in the ranges tested. Limits of detection were 0.2 and 0.4 μg and limits of quantification were 0.5 and 1.0 μg for withaferin-A and 6-gingerol, respectively. Intra and inter-day RSD of retention times and peak areas were less than 2.1%. Recovery was between 94.5 and 98.8% for withaferin-A and 94.2 and 102.4% for 6-gingerol. The established HPLC method is appropriate and the two markers are well resolved, enabling efficient quantitative analysis of withaferin-A and 6-gingerol. The method was successfully used for quantitative analysis of these two marker constituents in a marketed polyherbal formulation.
Summary
Fourteen samples of fresh curry leaves (Murraya Koenigii) were collected from 13 states of India and analyzed for 6 minor (Ca, Cl, K, Mg, Na and P) and 14 trace (Br, Ce, Co, Cr, Cs, Fe, Hg, Mn, Rb, Sb, Sc, Se Th and Zn) elements by 2-minute irradiation in a reactor followed by high resolution g-ray spectrometry. Peach Leaves (SRM-1547) and Mixed Polish Herbs (MPH-2) were used as comparator standards. Phosphorus was determined by counting the b-activity from 32P using an end-window GM counter. Most elements were found to vary in a wide range depending on their origin of location, e.g., Na (104-455 mg/g), K (10.3-30.3 mg/g), Ca (9.44-28.3 mg/g), Mg (1.14-7.19 mg/g), P (0.43-1.69 mg/g), Mn (24.8-63.0 mg/g), Fe (72.5-195 mg/g), Se (40.1-131 ng/g) and Zn (7.90-70.5 mg/g). Variation in the elemental concentrations of the same species of different origin may be attributed to ecological and geographical variations. Further, column and thin layer chromatography were used for separating three organic constituents from the ethanolic extract; 3-methylthiopropanenitrile; 1,2-benzenedicarboxylic acid, mono (2-ethylhexyl ester) and 1-penten-3-ol and characterized by IR and GC-MS. Inorganic elements may be present as complexes with the organic compounds.
Research over the last few years has shown that inoculation with nitrogen-fixing bacteria of the genus Azorhizobium presents an alternative for (or supplement to) chemical fertilization, mainly due to the capability of the bacteria to produce plant growth- promoting hormones. The Azorhizobium caulinodans strain ORS 571 in combination with 2,4-D was able to colonize the root interior of an Indian maize cultivar. After transplanting to pots, it was noticed that nodulated and Azorhizobium -treated plants showed higher chlorophyll content in the leaf and enhanced nitrate reductase activity, leading to higher yield as compared to the control plants (non-nodulated). A plant growth-promoting effect was clearly visible in all inoculated plants examined. nodulated plants treated with Azorhizobium had higher physiological activities as compared to plants treated only with Azorhizobium . Azorhizobium therefore creates potentially better symbiosis in the form of para -nodules and promotes a higher level of nitrogen fixation, leading to better growth and plant development, with reduced requirements for chemical fertilizers.
Abstract
A direct evaporation method is described for the preparation of sources using stainless steel as the backing material and tetraethylene glycol (TEG) as a spreading agent in the presence of large amounts of uranium. It is shown that FWHM and tail contribution at the low energy peak due to energy degradation of the high energy peak can be optimized by heating the source under controlled conditions in a furnace at 500–600°C for about 15 min. An accuracy of 0.5–1% is demonstrated for the determination of238Pu/(239Pu+240Pu) alpha activity ratio in the U/Pu range of 10 to 1500 generally encountered in dissolver solution of irradiated fuel.
Abstract
A method is described for the determination of plutonium concentration in the presence of a bulk of other impurities by isotope dilution mass spectrometry /IDMS/ using239Pu as a spike. The method involves the addition of239Pu spike /
90 atom%/ to samples with239Pu /
70 atom%/ and vice versa. After ensuring chemical exchange between the sample and the spike isotopes, plutonium is purified by conventional anion exchange procedure in 7M HNO3 medium.239Pu/240Pu atom ratio in the purified spiked sample is determined with high precision /better than 0.1%/ using a thermal ionization mass spectrometer. Concentration of plutonium in the sample is calculated from the changes in239Pu/240Pu atom ratio in the spiked mixture. Results obtained on different plutonium samples using239Pu as a spike are compared with those obtained by the use of242Pu spike. Precision and accuracy comparable to those achieved by using242Pu are demonstrated. The method provides an alternative in the event of non-availability of enriched242Pu or244Pu required in IDMS of plutonium and at the same time, offers certain advantages over the use of242Pu or244Pu spike.
Abstract
A reverse isotope dilution alpha spectrometric /R-IDAS/ method using239Pu as a spike is described for the determination of plutonium concentration in high burn-up fuel samples wth238Pu/(239Pu+240Pu) alpha activity ratio >0.5, without resorting to any purification from241Am and a bulk of other impurities. It involves the addition of a pre-clibrated spike solution to a known aliquot of the plutonium sample solution followed by source preparation using TEG as a spreading agent. The results obtained on a number of plutonium samples containing 20–80% of241Am /alpha activity wise/ using this method are compared with those achieved by R-IDAS using purification with TTA, with respect to precision and accuracy. Precision and accuracy of 0.5% are demonstrated. This method eliminates the need of any separation and purification of plutonium from241Am and a bulk of other impurities like uranium.
Ninety-nine wheat cultivars from six different agro-climatic zones of India were analyzed for the Vrn-1, Vrn-2, Vrn-B3, Vrn-4 and Ppd-D1 composition with DNA sequenced based allele specific or linked markers for the above-mentioned genes. A majority of the germplasm carried the dominant Vrn-A1a allele alone or in combination with Vrn-B1 and Vrn-D1. The three dominant genes were cumulatively present in 30 cultivars among all the zones, whereas double dominant combination, Vrn- A1/Vrn-B1 was identified in 18 cultivars, Vrn-A1/Vrn-D1 in 6 cvs and Vrn-B1/Vrn-D1 in 16 cvs. The combination of the dominant alleles of all three genes was most frequent in cvs of Northern Western Plains Zone. Northern Hill Zone had vrn-B1 and vrn-D1 alleles in higher proportions compared to the dominant alleles Vrn-B1 and Vrn-D1 indicating successful spring/winter wheat cross breeding. All of the cvs had the recessive Vrn-B3 allele. Most of the cvs had photoperiod insensitive allele in all the zones and only 9% cvs possessed the photoperiod sensitive allele (b) of the Ppd-D1 gene. This information will be useful in selecting parental lines for crossing to maximize diversity at these loci and for future molecular marker assisted breeding for cultivar improvement.
Abstract
A hot vacuum extraction technique for the determination of hydrogen in metal and alloy samples has been standardised. After measuring the total pressure of the evolved gases, individual hydrogen and deuterium intensities are measured using an on-line quadrupole mass spectrometer. Synthetic mixtures of H2 and D2, in known concentrations, have been analysed by QMS and an analytical expression correlating the measured [D2]/[HD] intensity ratio with the mole fraction of deuterium in the synthetic mixture has been arrived at. The precision and accuracy in the measurement of hydrogen is about 10% at 50 ppmw level.
Abstract
K-factors (= certified isotope ratio/observed isotope ratio) are determined for the isotope abundance measurements of uranium and plutonium by thermal ionisation mass spectrometry. An mdf of 0.07% and 0.18% per mass unit differing by a factor of about 3, is obtained for uranium and plutonium, respectively, employing double rhenium filament assembly in the ion source and Faraday cup as the detector using the presently available isotopic reference materials of uranium and plutonium.
