Xie Yunfei, Luo Tian, Yang Jing, Dong Yuming
Lanzhou University, School of Pharmacy, Institute of Pharmaceutical Analysis, Lanzhou 730000, People's Republic of China.
J AOAC Int. 2018 Jan 1;101(1):249-255. doi: 10.5740/jaoacint.17-0103. Epub 2017 Jul 31.
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%.
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%。