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.
作者
励炯
曹青文
胡宏宇
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)
出处
《分析科学学报》
CAS
CSCD
北大核心
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)。
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)
Ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
Column solid phase extraction
Infant formula
Quaternary ammonium compounds(QACs)
