UPLC-MS测定不同产地薏苡仁中甘油三油酸酯的含量

Determination of Triolein Content in Coicis Semen from Different Regions by UPLC-MS

关键词:  UPLC-MS  薏苡仁  甘油三油酸酯  质量控制

Key words:  UPLC-MS  Coicis Semen  triolein  quality control

摘要:

目的 建立测定甘油三油酸酯的UPLC-MS，并对23个不同产地的薏苡仁中甘油三油酸酯含量进行测定。方法 使用Waters Quattro Micro液质联用仪，色谱柱为Acquity UPLC BEH C₁₈柱(2.1 mm×100 mm，1.7 μm)；流动相(A)为甲醇-乙腈-氨水(19∶19∶2)调至pH 3的0.1%甲酸溶液，流动相(B)为异丙醇，A-B(55∶45)；柱温45 ℃；流速0.3 mL·min^-1；ESI+，多反应监测模式，监测离子为m/z 902.8→m/z 603.2。结果 标准曲线为Y=4.233×103X+ 9.172×102(r=0.999 5)，甘油三油酸酯在0.142~25.56 μg·mL^-1内具有良好的线性关系；平均回收率为97.21%，RSD为1.44%(n=9)；不同产地来源薏苡仁中甘油三油酸酯含量存在差异。结论 本方法灵敏、准确、重复性好，可用于薏苡仁及薏苡仁油的质量控制。

Abstract:

OBJECTIVE To establish a ultra-high performance liquid chromatography with mass(UPLC-MS) method for determination of triolein content, and determine triolein content in Coicis Semen from 23 different regions. METHODS Using Waters Quattro Micro with mass, the column was Acquity UPLC BEH C₁₈(2.1 mm×100 mm, 1.7 μm); the mobile phase was made up that A phase contained methanol, acetonitrile and 0.1% formic acid solution with ammonia to pH 3 in the proportion for 19∶19∶2, and B phase was isopropyl alcohol, the proportion of A phase and B phase was 55∶45; column temperature was 45 ℃; the flow rate was 0.3 mL·min^-1. Detection in ESI using positive ionization and multiple reactions monitoring mode(MRM) was applied to determine positive ions m/z 902.8→m/z 603.2. RESULTS The standard curve was Y=4.233×103X+9.172×102(r=0.999 5), the tirolein in linear range of 0.142-25.56 μg·mL^-1 had a good linear relationship; the average recovery was 97.21%, RSD was 1.44%(n=9); and triolein content in Coicis Semen from different regions was different. CONCLUSION The established UPLC-MS method on determination of triolein content in Coicis Semen is sensitive, rapid, accurate, reproducible and can be used for the quality control of Coicis Semen.