食品中季铵盐类消毒剂检测方法建立及北京市市售食品及膳食样品中含量分析

Development of a Detection Method for Quaternary Ammonium Compounds in Foods and Its Application to Commercial Foods and Dietary Samples in Beijing

建立了一种基于超高效液相色谱-串联质谱检测蔬菜、水果、水产等多种食品基质中9种常用季铵盐类消毒剂的分析方法。样品采用改良的QuEChERS(Quick、Easy、Cheap、Effective、Rugged、Safe)法净化,BEH C_(18)色谱柱(100 mm×3.0 mm,1.7μm)分离,电喷雾电离质谱正离子模式下分析。方法学考察结果表明,蔬菜、水果、水产中9种季铵盐的检出限为0.2~5.0μg/kg,定量限为1.0~10.0μg/kg,在各自的检测范围内有良好的线性关系(R^(2)>0.99),平均回收率为65.24%~118.63%,相对标准偏差为0.19%~6.77%。使用本方法检测北京市市售食品季铵盐含量,阳性样品检出率为30.43%;检测北京市膳食样品季铵盐含量,阳性样品检出率为12%,膳食摄入风险在可接受范围内。

An analytical method based on ultra-high performance liquid chromatography-tandem mass spectrometry was developed for the simultaneous detection of nine commonly used quaternary ammonium compounds(QACs)in various food matrices including vegetables,fruits,and aquatic products.The enrichment and purification of QACs were achieved using an improved quick,easy,cheap,effective,rugged and safe(QuEChERS)method,and the separation was performed on a BEH C18 column(100 mm×3.0 mm,1.7μm)with gradient elution.QACs were detected using an electrospray ionization source in the positive ion mode.The limits of detection and quantification for the nine QACs in vegetables,fruits,and aquatic products were 0.2–5.0 and 1.0–10.0μg/kg,respectively,and good linearity was observed for all analytes within their respective concentration ranges(R^(2)>0.99).The recoveries for spiked samples were in the range of 65.24%–118.63%with relative standard deviations(RSDs)of 0.19%–6.77%.When the developed method was applied to commercial foods and dietary samples in Beijing,detection rates of 30.43%and 12%were obtained,respectively.The dietary risk of QAC residues was acceptable.