固相萃取-气相色谱-质谱法测定酱油中3-氯-1,2-丙二醇

Determination of 3-Mono-chloropropane-1,2-diol in Soy Sauce by Solid Phase Extraction with Gas Chromatography-Mass Spectrometry

建立了酱油中3-氯-1,2-丙二醇(3-MCPD)残留量的固相萃取-气相色谱-质谱(GC/MS)分析方法。利用SampliQ OPT固相萃取柱净化样品,考察了乙醇、丙酮、乙醚、乙醚-正已烷(9:1,V/V)4种洗脱液对3-MCPD回收效果的影响。洗脱液在室温下经氮气吹干后用双(三甲基硅烷基)三氟乙酰胺-三甲基氯硅烷(BSTFA-TMS,99:1,V/V)衍生,采用气相色谱质谱的选择离子模式(SIM:m/z116,147)进行定量测定。本方法的检出限为0.1μg/L,添加浓度在0.025～0.1μg/g范围内,平均回收率为96%～102%,相对标准偏差(RSD)为1.6%。衍生物的峰面积与浓度在5.0～100.0μg/L范围内呈良好的线性关系(r=0.9984)。

A novel method was developed for the determination of trace 3-mono-chloropropane-1,2diol（3-MCPD） in soy sauce by solid phase extraction with gas chromatography-mass spectrometry.The sample was clarified by SampliQ OPT solid extraction column.Four kinds of eluent solvent（ethanol,acetone,ether,ether-hexane） affecting on recoveries of 3-MCPD were examined.The eluent was derivated with trimethyl chlorosilane and bis（trimethylsilyl） trifluoroacetamide（BSTFA-TMS,99：1,V/V） after it was dried by nitrogen in room temperature.The selected ion mode（SIM） detection method（ions elected：m/z 116 and 147） was used for the detection of the 3-MCPD derivative.The detection limit was 0.1μg/L for 3-MCPD.The sample average recoveries were 96%-102% in 0.025-0.1μg/g and the relative standard deviation was 1.6%.There was a good linear correlation（r = 0.9984） between the peak areas and concentration of derivative in the range of 5.0-100μg/L.