作　　者： ; ; ; ; ; ; ; ; ;

机构地区： 中国广州分析测试中心

出　　处： 《分析测试学报》 2012年第2期143-147,共5页

摘　　要： 建立了气相色谱-串联质谱同时测定调味品中1,3-二氯-2-丙醇(1,3-DCP)、2,3-二氯-1-丙醇(2,3-DCP)和3-氯-1,2-丙二醇(3-MCPD)的分析方法。优化了样品前处理方法及GC-MS/MS分析条件,结果显示,样品经硅藻土净化,正己烷-乙醚(5∶5)洗脱,三氟乙酸酐衍生化后,在GC-MS/MS多反应监测模式(MRM)下测定,3种氯丙醇在0.001～10 mg/L范围内呈良好线性,相关系数分别为0.999 8、0.999 6和0.999 7;检出限(S/N=3)均为0.000 5 mg/kg,加标回收率为88%～97%。该方法简便、快速、溶剂用量少、衍生化试剂价廉易得,且能消除调味品中复杂基质的干扰,结果准确可靠、灵敏度高,适用于调味品中3种氯丙醇的同时测定。 A method was developed for the determination of 1,3-dichloro-2-propanol（1,3-DCP）,2,3-dichloro-1-propanol（2,3-DCP） and 3-chloro-1,2-propanediol（3-MCPD） in condimen by gas chromatography-tandem mass spectrometry（GC-MS/MS）.The conditions for sample pretreatment and GC-MS/MS were investigated and optimized.The samples were purified by kieselguhr,eluted with hexane-diethyl ether（5 ∶ 5）,then derivatised by trifluoroacetic acid anhydride.The detection was carried out by GC-MS/MS in the multiple-reaction monitoring（MRM） mode.Good linear relationships of three analyte were obtained in the concentration range of 0.001-10 mg/L,with correlation coefficients of 0.999 8,0.999 6 and 0.999 7,respectively.The limits of detection were all 0.000 5 mg/kg（S/N=3）,and the recoveries ranged from 88% to 97%（n=6）.This method is simple,rapid,low solvent consumption,cheap price of derivative,and the complex matrix disturbance in condimen samples was diminished when MRM mode was adopted.The accuracy,reliability and sensitivity of the method made it was suitable for the determination of three chloropropanols in condimen samples.

关 键 词： 气相色谱 串联质谱法 调味品 二氯 丙醇 二氯 丙醇 氯 丙二醇 多反应监测模式

领　　域： [理学] [理学] [理学] [理学]