气相色谱法检测汤料中氯丙醇类化合物
Gas Chromatographic Determination of Chloropropanols in Stocks
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摘要: 应用毛细管柱-气相色谱法测定汤料中氯丙醇类化合物.汤料试样中氯丙醇类化合物在索氏抽取器中用乙醚萃取,于萃取液中通入氮气吹干乙醚,残留物用每次1 mL甲醇萃取两次以净化氯丙醇类化合物.收集并合并甲醇萃取液,蒸发除去甲醇后用N,O-双(三甲基硅烷)-三氟乙酰胺进行衍生化,所得衍生物经毛细管色谱柱分离,用氢火焰离子化检测器(FID)检测,方法的检出限为0.01 mg·kg-1.对精密度及回收率作了试验,得到的回收率在95%~102%之间,RSD(n=5)值小于4.5%.Abstract: Gas chromatography with capillary column was applied to the determination of chloropropanols in stocks.Chloropropanols in the stock sample was extracted with ethyl ether using Soxhlet apparatus,and the ethyl ether was evaporated by nitrogen stream.The chloropropanols were then purified by extraction with methanol twice in 1 mL portions.The extracts were collected and methanol was evaporated,and derivatized with N,O-bis(trimethylsilyl)-trifluoroacetamide (BSTFA).The derivatives was separated on the capillary chromatographic column and determined by flame ionization detection.Detection limit of the method was 0.01 mg·kg-1.Tests for recovery and precision were done giving values of recovery in the range from 95% to 102%,and RSD′s (n=5) less than 4.5%.