摘要
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.
出处
《分析测试学报》
CAS
CSCD
北大核心
2014年第1期108-111,共4页
Journal of Instrumental Analysis
基金
科技部973计划(2012CB720804)
关键词
氨基甲酸乙酯
酱油
食醋
气相色谱-质谱法
分散固相萃取
ethyl carbamate
soy sauce
vinegar
gas chromatography-mass spectrometry (GC-MS)
dispersive solid phase extraction(d-SPE)