通过式固相萃取-气相色谱-串联质谱法测定动物源性食品中11种N-亚硝胺类化合物

选取通过式固相萃取技术，结合气相色谱-串联质谱法（gas chromatography-tandem mass spectrometry,GC-MS/MS），建立动物源性食品中11种N-亚硝胺类化合物的分析方法。样品加水浸泡后采用乙腈提取，经Prime HLB通过式固相萃取柱（200 mg/6 mL）快速净化，采用多反应监测模式监测，以空白基质匹配标准溶液外标法定量。结果表明：11种N-亚硝胺类化合物在0.5～500.0 ng/m L范围内线性关系良好，相关系数为0.999 4～0.999 8，检出限为0.2～0.3μg/kg，定量限为0.5～1.0μg/kg；在1、4、10μg/kg 3个加标水平下，11种N-亚硝胺类化合物平均加标回收率为80.1%～97.4%，相对标准偏差为2.3%～8.8%；该方法提取及净化时间仅需15 min/样品，与GB 5009.26—2016《食品安全国家标准食品中N-亚硝胺类化合物的测定》方法相比，提取与净化时间大幅缩短，检测效率提升10倍，可实现动物源性食品中N-亚硝胺类化合物的快速测定。

Determination of Eleven N-Nitrosamines in Animal Derived Foods by Gas Chromatography-Tandem Mass Spectrometry after Pass-Through Solid Phase Extraction

A method was developed for the determination of 11 N-nitrosamines in animal derived foods by pass-through solid phase extraction coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS). The rehydrated samples were extracted with acetonitrile and rapidly purified by using a Prime HLB solid phase extraction column (200 mg/6 mL). The target compounds were detected in the multiple reaction monitoring (MRM) mode, and quantified by the matrix matched external standard method. The calibration curves for the 11 N-nitrosamines were linear in the concentration range of 0.5–500.0 ng/mL, with correlation coefficients of 0.999 4–0.999 8. The limits of detection (LODs) and the limits of quantitation (LOQs) were 0.2–0.3 and 0.5–1.0 μg/kg, respectively. The average recoveries at spiked levels of 1, 4 and 10 μg/kg ranged from 80.1% to 97.4%, and the relative standard deviations (RSDs) were between 2.3% and 8.8%. The extraction and purification time required by this method was only 15 min/sample and greatly shortened compared with GB 5009.26-2016, and the detection efficiency was increased by 10 times. This method allows rapid detection of N-nitrosamines residues in animal derived foods.