目的:建立一种简单、快速、可同时检测22种氨基酸的色谱方法,并利用此方法对树莓中的游离氨基酸进行检测和分析,为树莓的开发提供科学依据。方法:以2,4-二硝基氟苯为柱前衍生试剂,Hypersil ODS2色谱柱,流动相A为40 mmol/L p H 6.4乙酸...目的:建立一种简单、快速、可同时检测22种氨基酸的色谱方法,并利用此方法对树莓中的游离氨基酸进行检测和分析,为树莓的开发提供科学依据。方法:以2,4-二硝基氟苯为柱前衍生试剂,Hypersil ODS2色谱柱,流动相A为40 mmol/L p H 6.4乙酸钠溶液,流动相B为体积分数50%乙腈-水溶液,梯度洗脱,反相高效液相色谱,二极管阵列检测器,检测波长360 nm。结果:22种氨基酸线性方程的相关系数范围为0.993 1~1.000 0,相对标准偏差在0.95%~4.98%之间,加标回收率为97.10%~103.39%,最低检出限为0.39~2.87μg/m L,定量限为1.29~9.47μg/m L。利用所建方法检测出树莓中含有14种游离氨基酸,其中6种人体必需氨基酸,占总氨基酸含量的29.36%。结论:所建方法操作简便、重复性好,树莓氨基酸含量丰富,有开发价值。展开更多
A reversed-phase High Performance Liquid Chromatography method is developed for the determination of fenfluramine in slimming drug using precolumn derivatization.After eluted with chloroform,the samples were derivatiz...A reversed-phase High Performance Liquid Chromatography method is developed for the determination of fenfluramine in slimming drug using precolumn derivatization.After eluted with chloroform,the samples were derivatized in solution of acetonitrile with water by 2,4-dinitrofluorobenzene at 40℃ for 60min in presence of Na2CO3 catalyst.The derivative obtained was determined on a Kromasil C18 column by using methanol-water （78:22,v/v） as mobile phase,and detection at 365 nm.The calibration curve is well linear in the range from 1.71～85.6 μg/mL with 0.9987 of correlation coefficient.The recoveries of the method range from 90.6 to 98.0% with a relative standard deviation less than 4% and the limit of detection 1.02 ng （S/N=3）.展开更多
文摘A reversed-phase High Performance Liquid Chromatography method is developed for the determination of fenfluramine in slimming drug using precolumn derivatization.After eluted with chloroform,the samples were derivatized in solution of acetonitrile with water by 2,4-dinitrofluorobenzene at 40℃ for 60min in presence of Na2CO3 catalyst.The derivative obtained was determined on a Kromasil C18 column by using methanol-water （78:22,v/v） as mobile phase,and detection at 365 nm.The calibration curve is well linear in the range from 1.71～85.6 μg/mL with 0.9987 of correlation coefficient.The recoveries of the method range from 90.6 to 98.0% with a relative standard deviation less than 4% and the limit of detection 1.02 ng （S/N=3）.
