液-液萃取/气相色谱-质谱法快速测定酱油中的3-氯-1,2-丙二醇  

Rapid determination of 3-chloro-1,2-propanediol in soy sauce by liquid-liquid extraction and gas chromatography-mass spectrometry

作　　者：张敬波 Zhang Jingbo(Dalian Center for Certification and Food and Drug Control,Dalian 116630,China)

机构地区：[1]大连市检验检测认证技术服务中心,大连116630

出　　处：《分析仪器》2023年第1期39-43,共5页Analytical Instrumentation

摘　　要：建立了酱油中3-氯-1,2-丙二醇(3-MCPD)的液-液萃取/气相色谱-质谱联用(LLE/GC-MS)检测方法。丁酮作为提取溶剂同时也是衍生试剂。样品加入同位素内标并用氯化钠饱和后用丁酮进行提取,提取液经干燥和净化后加入对甲苯磺酸作催化剂进行衍生。衍生溶液经中和、干燥后用气相色谱-质谱联用仪在选择离子模式下进行测定。3-MCPD在0.008~2.0μg的含量范围内线性关系良好,相关系数(r)为0.9999,定量限为0.003 mg/kg。在添加水平0.005~0.40mg/kg时准确度为-8.2%~-1.7%,精密度(RSD)1.3%~3.7%。该方法操作简单,检测成本低且灵敏度高,成本低,选择性好,适用于酱油中的3-氯-1,2-丙二醇的快速测定。Butanone was chosen as extraction solvent and derivatization reagent.The sample was added with isotope internal standard(d5-3-MCPD)and saturated with sodium chloride,extracted with methyl ethyl ketone.The extract was dried and purified,with anhydrous magnesium sulfate and PSA.3-MCPD and d5-3-MCPD react with the solvent in the presence of p-toluenesulphonic acid.Neutralized by excess K_(2)CO_(3),the derived solution was dried and determined with GC-MS in selected ion monitoring mode(SIM).Good linear relationship of the analyte was obtained in the concentration range of 0.008—2.0μg,with correlation coefficient of 0.9999.The limits of quantitation was 0.003 mg/kg.The accuracy of 0.005—0.40 mg/kg was ranged from -8.2% to -1.7% and the relative standard deviations(RSD)were between 1.3%and 3.7%(n=6).It was a simple,quick,lowcost,high sensitive and reliable analysis method.

关 键 词：3-氯-1 2-丙二醇 酱油 液-液萃取 气相色谱-质谱联用法 

分 类 号：O657.63[理学—分析化学] TS264.21[理学—化学]