气相色谱-质谱联用法测定液体调味料中4种氯丙醇的含量

Determination of 4 kinds of chloropropanols in liquid condiment by GC-MS

选取酱油、鱼露与水解植物蛋白液为试验样品,建立了液体调味料中3-氯-1,2-丙二醇(3-MCPD)、2-氯-1,3-丙二醇(2-MCPD)、1,3-二氯-2-丙醇(1,3-DCP)和2,3-二氯-1-丙醇(2,3-DCP)的气相色谱-质谱联用(GC-MS)检测方法。以样品加入稳定同位素内标后进行固相支持液液萃取,以10 mL正己烷淋洗,15 mL乙酸乙酯洗脱,氮吹近干后,七氟丁酰基咪唑衍生,产物经DB-5MS柱分离,质谱采用选择离子监测模式检测。结果表明,四种氯丙醇在0.005~1.6μg/mL质量浓度范围内呈良好线性关系,3-MCPD、2-MCPD、1,3-DCP和2,3-DCP的检出限分别为2.0μg/kg、2.0μg/kg、5.0μg/kg、5.0μg/kg,定量限分别为5.0μg/kg、5.0μg/kg、10μg/kg、10μg/kg,加标回收率在82.4%~107.0%范围内,精密度实验结果的相对标准偏差(RSD)在0.85%~8.58%范围内。该方法前处理简便,定量准确可靠,可用于液体调味料中四种氯丙醇含量的检测。

Using soy sauce,fish sauce and hydrolyzed vegetable protein liquid as the test samples,the gas chromatography-mass spectrometry(GC-MS)method was established for the determination of 3-chloro-1,2-propanediol(3-MCPD),2-chloro-1,3-propanediol(2-MCPD),1,3-dichloro-2-propanol(1,3-DCP)and 2,3-dichloro-1-propanol(2,3-DCP)in liquid condiment.The solid-phase supported liquid-liquid extraction was conducted after the samples were added with stable isotope internal standard,then processed with 10 ml n-hexane leaching,15 ml ethyl acetate eluting,and nearly dried by nitrogen,sevoflurobuylimidazole derivatizing,the derivations were separated by DB-5MS column and detected by mass spectrometry selected ion mornitoring mode.The results showed that 4 kinds of chloropropanols had good linearity in the mass concentration range of 0.005-1.6μg/ml.The detection limit of 3-MCPD,2-MCPD,1,3-DCP and 2,3-DCP were 2.0μg/kg,2.0μg/kg,5.0μg/kg,5.0μg/kg,respectively.The quantitation limits were 5.0μg/kg,5.0μg/kg,10μg/kg,10μg/kg,respectively.The standard recovery rates were in the range of 82.4%-107.0%,and the relative standard deviations(RSD)of precision test results were in the range of 0.85%-8.58%.The method was simple in pretreatment,accurate and reliable,which could be used for the determination of 4 kinds of chloropropanol in liquid condiment.