A sensitive and accurate LC with tandem MS (MS/MS)-based method was developed and validated for the analysis of the herbicide glyphosate, its metabolite aminomethylphosphonic acid (AMPA), and glufosinate after derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl) in various plant matrixes. The method also covers direct analysis of the glufosinate metabolites 3-methylphosphinicopropionic acid (3-MPPA) and N-acetyl-glufosinate (NAG). The homogenized samples were extracted with 0.1% formic acid in water-dichloromethane (50 + 50). The aqueous layer was derivatized with FMOC-Cl, cleaned through an HLB SPE cartridge, and determined by LC-MS/MS. The sample size, extraction solvent, sample-to-solvent ratio, derivatization conditions, and cleanup procedure were thoroughly optimized, the LOQs of glyphosate, glufosinate, and AMPA were 0.5 ng/g in grape, corn (leaf and seed), and cotton (leaf, seed, and oil) and 2 ng/g in soybean and tea. The LOQs of NAG and 3-MPPA were 50 ng/g in all the test matrixes, except tea and soybean, for which the LOQ was 100 ng/g. In all cases, average recoveries were >80%. The method successfully performed the estimation of glyphosate in incurred corn and cotton leaf samples collected from supervised field trials.
The goal of the present study was to investigate the bioactive molecules (anthocyanins and fatty acids) present in the aril of pomegranate. Major anthocyanins present in the aril of pomegranate were identified by HRMS as delphinidin 3,5-diglucoside, cyanidin 3,5-diglucoside, pelargonidin 3,5-diglucoside, cyanidin 3-glucoside and delphinidin 3-glucoside. In-vitro study revealed that bioaccessibility of anthocyanin in duodenal condition was varied between 7.3 and 9.7%. Encapsulation enhances the bioaccessibility of both the phenolics to some extent in gastric as well as duodenal condition. Seed oil contains significant amount of unsaturated fatty acids especially ω-5 fatty acids. Geometrical isomers of ω-5 fatty acids were also identified by GC-MS. The spray dried anthocyanin formulation has potential for food application.
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