分散固相萃取/气相色谱-质谱法测定酱油及食醋中氨基甲酸乙酯

Determination of Ethyl Carbamate in Soy Sauce and Vinegar by Dispersive Solid Phase Extraction/Gas Chromatography-Mass Spectrometry

建立了分散固相萃取（d-SPE）/气相色谱-质谱法（GC-MS）检测酱油和食醋中氨基甲酸乙酯（EC）含量的分析方法.基于不同样品基质的复杂性,以乙腈（酱油）或者乙酸乙酯（食醋）进行液液萃取,经N-丙基乙二胺（PSA）分散固相萃取净化.考察了萃取溶剂的种类、萃取次数和PSA使用量等因素对EC萃取效率和分析效果的影响.在优化实验条件下,EC在10～500 μg/L质量浓度范围内呈良好的线性关系,线性系数（r2）为0.9998.EC在酱油和食醋两种基质中的定量下限均为5.0 μg/kg,不同加标水平下的平均回收率为92.9％～114.3％,相对标准偏差为0.5％～5.3％.该方法简单、灵敏、准确,适用于酱油和食醋中EC含量的测定,具有很好的实际应用价值.

A dispersive solid phase extraction （d-SPE）/gas chromatography-mass spectrometric （GC-MS） method for the determination of ethyl carbamate（EC） in soy sauce and vinegar was established.Based on the different sample matrix,the samples were processed by liquid-liquid extraction with acetonitrile（soy sauce） or ethyl acetate（vinegar）,and purified by dispersive solid phase extraction with N-propyl ethlene diamine （PSA）.Effects of solvent type,extraction times and PSA usage on extraction efficiencies and analytical results of EC were discussed.Under the optimal conditions,the method showed a good linearity in the range of 10-500 μg/L for EC with correlation coefficient（r2） of 0.999 8.The average recoveries of EC at different spiked levels were in the range of 92.9％-114.3％ with RSDs of 0.5％-5.3％.The quantitation limits for EC in soy sauce and vinegar were both 5.0 μg/kg.The result showed that the method was simple,sensitive and accurate,and was suitable for the determination of EC in soy sauce and vinegar.