氢氧化钡处理-二氯甲烷萃取/GC-MS/MS检测几种水产品和加工肉制品中的7种N-亚硝胺
Determination of 7 N-nitrosamines in Several Aquatic Products and Processed Meat Products by Gas Chromatography-tandem Mass Spectrometry with Barium Hydroxide Treatment Coupled Liquid-liquid Extraction
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摘要: 建立了氢氧化钡处理结合二氯甲烷萃取进行样品处理,气相色谱-串联质谱法检测几种水产品和加工肉制品中7种N-亚硝胺的新方法。以N-亚硝基二甲胺-d6、N-亚硝基二正丙胺-d14和N-亚硝基吡咯烷-d8为内标,10 g样品于50 mL离心管中经氢氧化钡溶液一步处理,离心后上清液再经二氯甲烷一次萃取,旋蒸浓缩至5 mL,氮吹至1 mL,DB-WAXUI柱(30 m×250 μm×0. 25 μm)进行色谱分离,多反应监测(MRM)模式进行质谱检测。该方法样品处理简便易行,7种N-亚硝胺在1~100 ng/mL浓度范围内线性良好(R2 > 0. 999);检出限为0.08~0.23 μg/kg,定量限为0.25~0.76 μg/kg;添加回收率为71.6%~133.8%,RSD为2.04%~17.1%。对市售9个鱼虾和8个加工肉制品的实际检测显示,N-亚硝基二甲胺的含量均在安全范围内。Abstract: A new method for determination of 7 N-nitrosamines in several aquatic products and processed meat products was developed by gas chromatography-tandem mass spectrometry (GC-MS/MS) with barium hydroxide treatment combined with dichloromethane extraction. With N-nitrosodimethylamine-d6,N-nitrosadipropylamine-d14 and N-nitrosopyrrolidine-d8 as internal standards,total 10 g sample was treated with the barium hydroxide solution in a centrifuge tube of 50 mL and centrifuged,then the supernatant was extracted with dichloromethane one time and the extraction was concentrated to 5 mL with a rotary vacuum evaporator and was next concentrated to 1 mL by nitrogen gas blowing. The chromatographic separation was carried with a DB-WAXUI column (30 m×250 μm×0.25 μm) and the mass spectrometry detection was done with multiple reactions monitoring mode. The calibration curves showed good linearity (1~100 ng/mL) with R2>0.999;the detection limits were 0.08~0.23 μg/kg and the quantitative limits were 0.25~0.76 μg/kg;the recoveries were 71.6%~133.8% with the relative standard deviations of 2.04%~17.1%. The actual test of nine dried fish and shrimp meat and eight processed meat products showed that the content of N-nitrosodimethylamine was within the safe range.