通过式固相萃取-超高效液相色谱-串联质谱法测定婴幼儿配方奶粉中的10种季铵盐类消毒剂残留  

Analysis of 10 Quaternary Ammonium Compounds in Infant Formula by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry After Solid Phase Extraction

作　　者：励炯[1,2] 曹青文 胡宏宇[1,2] 闫金花 金朦娜 LI Jiong;CAO Qingwen;HU Hongyu;YAN Jinhua;JIN Mengna(Hangzhou Institute for Food and Drug Control,Hangzhou 310017;Laboratory of Milk and Dairy Regulatory Technology of Zhejiang Provincial Administration for Market Regulation,Hangzhou 310017)

机构地区：[1]杭州市食品药品检验研究院,浙江杭州310017 [2]浙江省市场监督乳及乳制品监管技术重点实验室,浙江杭州310017

出　　处：《分析科学学报》2023年第4期424-430,共7页Journal of Analytical Science

基　　金：浙江省市场监管系统科研计划项目(ZC2021B049)。

摘　　要：建立了通过式固相萃取净化-超高效液相色谱-串联质谱法测定婴幼儿配方奶粉中的10种季铵盐类消毒剂(QACs)残留的方法。样品经水溶解后,用含0.2%甲酸的乙腈提取,提取液用甲醇1∶1混匀,用通过式固相小柱(Oasis PRiME HLB)净化,流动相由含0.2%甲酸的甲醇-乙腈溶液(体积比,6∶4)与含0.2%的甲酸水溶液组成。10种QACs在Waters CORTECS UPLC C18(100 mm×2.1 mm,1.6μm)色谱柱上以梯度洗脱分离后,采用电喷雾离子源正离子(ESI+)模式电离,配合多反应监测模式(MRM)进行定性定量分析。结果表明,10种QACs在各自浓度范围内线性良好,相关系数r^(2)≥0.9964,方法定量限(LQD)为0.5~3.0μg/kg。采用低、中、高3个浓度水平进行加标实验,回收率范围为86.2%~103.4%。方法简单高效,可作为日常婴幼儿配方奶粉监督抽样中10种季铵盐类消毒剂(QACs)残留检测的有效方法。A column solid phase extraction method for the determination of 10 quaternary ammonium compounds(QACs)residues in infant formula with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was optimized.The samples were dissolved in water and extracted with acetonitrile containing 0.2%(V/V)formic acid,and the extracts were mixed with 1∶1 methanol and cleaned up with a solid-phase extraction cartridge(Oasis PRiME HLB).10 QACs were analyzed by Waters CORTECS UPLC C18(100×2.1 mm,1.6μm)column with gradient elution,with the mobile phases consisting of methanol-acetonitrile solution(6∶4)containing 0.2%and aqueous solution containing 0.2%formic acid.10 target compounds were ionized in ESI+mode,together with MRM for qualitative and quantitative analysis.The results showed that the linearity of the 10 QACs was good with r^(2)≥0.9964;the spiked experiments were performed by using three concentration levels of low,medium and high,and the recoveries were in the range of 86.2%-103.4%;the limits of quantitative(LQD)were 0.5-3.0μg/kg.The method is simple and efficient with high recoveries and good reproducibility,and can be used for the detection of 10 quaternary ammonium compounds(QACs)residues in infant formula.

关 键 词：超高效液相色谱-串联质谱 通过式固相萃取 婴幼儿配方奶粉 季铵盐类消毒剂(QACs) 

分 类 号：O657.63[理学—分析化学]