分散固相萃取-同位素稀释-气相色谱-质谱法测定酱油中5种N-亚硝胺  

Simultaneous determination of five N-nitrosamines in soy sauces by dispersive solid-phase extraction and isotope dilution-gas chromatographymass spectrometry

作　　者：姚瑞雄 

机构地区：[1]广州出入境检验检疫局,广州510623

出　　处：《分析试验室》2018年第2期183-187,共5页Chinese Journal of Analysis Laboratory

摘　　要：应用分散固相萃取技术和同位素稀释技术,结合气相色谱-质谱仪(GC-MS),建立了同时测定酱油中5种挥发性N-亚硝胺(NAs)的分析方法。酱油样品采用乙酸乙酯提取,提取液经缓慢氮吹浓缩后,分散固相萃取净化,INNOWAX极性毛细管色谱柱分离,GC-MS选择离子扫描(SIM)模式分段检测,同位素内标法定量。方法学评价表明,5种NAs在质量浓度2.0~200μg/L范围内线性关系良好,相关系数均大于0.998;方法检出限为0.5~1.0μg/kg,定量限为1.5~3.0μg/kg;阴性酱油样品中3个添加水平的平均回收率为81.2%~115%,相对标准偏差(RSD)为3.0%~7.8%。方法应用于38个酱油样品的检测结果显示,有5个样品检出N-亚硝基哌啶(NPIP)。A sensitive and rapid method was established for simultaneous determination of five N- nitrosamines （NAs） in soy sauce by dispersive solid-phase extraction （dSPE） and isotope dilution-gas chromatography-mass spectrometry （GC-MS）. The samples were firstly extracted by ethyl acetate, then the extracting solution was concentrated by gentle nitrogen gas and subsequently purified with dSPE. All targets were separated by INNOWAX capillary chromatographic column, detected by selected ion monitoring （SIM） mode of GC-MS and quantified by isotope internal standard method. Under the optimized condition, the specificity of this method was favorable. The matrix effects of target analytes in soy sauce could be ignored. The linear range was 2. 0 -200 μg/L for five analytes with the correlation coefficients greater than 0. 998. The limits of detection （LODs） and the limits of quantitation （ LOQs ） of the developed method were 0. 5 - 1.0 μg,/kg and 1.5 - 3.0 μg/kg, respectively. The average recoveries of five NAs at three spiked levels in negative soy sauce were in the range of 81.2% -115% with relative standard deviation （RSD） of 3.0% -7.8%. The method was simple and rapid with good repeatability, and was successfully applied to analyze 38 soy sauces and N- nitrosopiperidine （NPIP） was detected in 5 samples.

关 键 词：N-亚硝胺 酱油 气相色谱-质谱法 分散固相萃取 

分 类 号：TS207.5[轻工技术与工程—食品科学]