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高效液相色谱梯度洗脱法快速测定啤酒、红酒和阿胶中的氨基酸:从胶束液相色谱到高亚胶束液相色谱

Rapid Determination of Amino Acids in Beer, Red Wine, and Donkey-Hide Gelatin by Gradient Elution of HPLC: From Micellar Liquid Chromatography to High Submicellar Liquid Chromatography.

作者信息

Xie Yunfei, Luo Tian, Yang Jing, Dong Yuming

机构信息

Lanzhou University, School of Pharmacy, Institute of Pharmaceutical Analysis, Lanzhou 730000, People's Republic of China.

出版信息

J AOAC Int. 2018 Jan 1;101(1):249-255. doi: 10.5740/jaoacint.17-0103. Epub 2017 Jul 31.

Abstract

Amino acids (AAs) in beer, red wine, and donkey-hide gelatin were rapidly determined by gradient LC elution from micellar LC to high submicellar LC. Mobile phase A was a 0.075 M sodium dodecyl sulfate solution containing 20 mM ammonium acetate with a pH value adjusted to 3.5 with acetic acid solution, and mobile phase B was acetonitrile. Optimized chromatographic conditions were as follows: mobile phase B increased from 25 to 60% (v/v) in 30 min and the use of a Venusil XBP C18 column (5 µm, 250 × 4.6 mm) as the stationary phase, with a column temperature of 35°C, flow rate of 1.2 mL/min, and detection wavelength of 266 nm. The results indicated good linearity (r2 ≥ 0.9924). The intraday precision of the retention time was RSD ≤ 1.1%, whereas interday was RSD ≤ 3.2%; intraday precision of the peak area was RSD ≤ 3.3%, whereas interday was RSD ≤ 4.9%. The range of recovery was 94.6-102.4%. The RSDs of the retention time for the AAs for the different samples were 0.04-0.31%.

摘要

采用从胶束液相色谱到高亚胶束液相色谱的梯度液相色谱洗脱法,快速测定啤酒、红酒和阿胶中的氨基酸。流动相A为含20 mM醋酸铵的0.075 M十二烷基硫酸钠溶液,用醋酸溶液将pH值调至3.5,流动相B为乙腈。优化的色谱条件如下:流动相B在30分钟内从25%(v/v)增加到60%,使用Venusil XBP C18柱(5 µm,250×4.6 mm)作为固定相,柱温35°C,流速1.2 mL/min,检测波长266 nm。结果表明线性良好(r2≥(0.9924))。保留时间的日内精密度RSD≤1.1%,日间精密度RSD≤3.2%;峰面积的日内精密度RSD≤3.3%,日间精密度RSD≤4.9%。回收率范围为94.6 - 102.4%。不同样品中氨基酸保留时间的RSD为0.04 - 0.31%。

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