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 UPLCBEH C18柱（2．1mm×100mm，1．7μm）；流动相（A）为甲醇-乙腈-氨水（19：19：2）调至pH3的0．1％甲酸溶液，流动相（B）为异丙醇，A—B（55：45）；柱温45℃；流速0．3mL·min^-1；ESI^＋，多反应监测模式，监测离子为m／z902．8→m／z603．2。结果标准曲线为Y=4．233×10^3X＋9．172×10^2（r=0．9995）。甘油三油酸酯在0．142-25．56pg·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。
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.
出处
《中国现代应用药学》
CAS
CSCD
2014年第2期200-204,共5页
Chinese Journal of Modern Applied Pharmacy
基金
福建省科技计划项目(2010Y2004)
