摘要
采用同位素内标法，建立气相色谆三重串联四极杆质谱测定火锅添加剂产品中3种氯丙醇的分析方法。样品加入氯丙醇的同位素内标，采用改良层析柱法（玻璃注射器．真空抽气系统）进行净化，正己烷．乙醚（1：1，V／V）进行提取，固相萃取法浓缩和富集，三氟乙酸酐衍生，以HP．5ms毛细管柱分离，串联四级杆质谱多反应监测模式检测，内标法定量。结果表明：采用本文的优化条件，用2种同位素内标（1，3-二氯-2-丙醇-d5和3-氯-1，2-丙二醇．d5）校正，可准确测定火锅添加剂产品中3种氯丙醇含量。在50-1000μg／L的范围内，方法线性良好，相关系数均可达0．999以上，方法回收率在82．5～104．0％之间，RSD小于5％。本方法灵敏、定量准确、衍生化试剂价廉易得，适用于火锅添加剂中3种氯丙醇的测定。
A new method was developed to determine three kinds of chloropropanols in chafing dish additives by gas chromatography with tandem mass spectrometry （GC-MS/MS） using isotope dilution technique. After spiked with isotope internal standards, the samples were eluted by chromatographic column, extracted with hexane and ether （1：1, V/V）, and then purified by solid phase column （SPE）. Trifluoroacetic anhydride （TFAA） was used as derivating agent. The targeted compotmds were determined by GC-MS/MS and quantified by internal standard method. Under the optimized condition, the method could be accurately to simultaneously determine three kinds of chloropropanols in chafing dish additives products with two kinds of internal standards （1,3-dichloro-2-propanol-d5 and 3-chloropropane-1, 2-diol-ds） for calibration . Within the linear range of 50 to 1000μg/L, the correlation coefficients were up to 0.999. The recoveries rates were between 82.5% and 104.0% with RSD less than 5% （n=6）. This method is sensitive, accuracy, and the derivative agent is inexpensive, which is suitable for determining three kinds of chloropropanols in chafing dish additives.
出处
《现代食品科技》
EI
CAS
北大核心
2014年第3期227-232,共6页
Modern Food Science and Technology
基金
广东省科技计划项目(2011B031500028)
