气相色谱-质谱联用法测定腌制水产品中的挥发性N-亚硝胺类化合物

Determination of volatile N-nitrosamine compounds in salted aquatic products by gas chromatography-mass spectrometry

建立了气相色谱-质谱(GC-MS)快速测定腌制水产品中挥发性N-亚硝胺含量的分析方法。采用GC-MS测定了N-二甲基亚硝胺(NDMA)、N-二乙基亚硝胺(NDEA)、N-二丙基亚硝胺(NDPA)、N-亚硝基吡咯烷(NPYR)、N-亚硝基哌啶(NPIP)、N-二丁基亚硝胺(NDBA)6种化合物,考察了样品不同提取方法、不同固相萃取小柱、不同色谱柱对分离检测的影响。结果显示:在10～1 000μg/L范围内,线性相关系数可达0.999 8以上;重现性良好,相对标准偏差小于8%;回收率可达79%～105%;灵敏度高,检出限低,除NDPA为0.03μg/kg外,其他5种N-亚硝胺为0.05μg/kg。该方法前处理快速简捷,易于操作,适用于腌制水产品中N-亚硝胺残留量的检测工作。

An analytical method was developed for the determination of the extraction of volatile N-nitrosamine compounds including N-nitrosodimethylamine （NDMA）, N-nitrosodiethylamine （NDEA） , N-nitrosodipropylamine （NDPA） , N-nitrosodibutylamine （NDBA） , N-nitrosopiperidine （NPIP）, and N-nitrosopyrrolidine （NPYR） from salted aquatic products by gas chromatography-mass spectrometry （GC-MS）. In this experiment, the separation and detection conditions were optimized for different extraction methods, solid-phase extraction columns, and chromatographic columns. The results showed that the linear correlation coefficients （R2 ） were higher than 0. 999 8 within l0 - I 000 μg/L, and the reproducibilities were good with the relative standard deviations （RSD） less than 8%. The recoveries were 79% - 105%. It is noted that this method for the determination of volatile N-nitrosamine compounds in salted aquatic products was much more sensitivity and with a lower detection limits （0.05 μg/kg except ND- PA） than the previously reported methods. This proposed method is rapid and convenient for the determination, and easy for the operation. It is appropriate for the determination of volatile N-nitrosamine compounds in various salted aquatic products.