分散固相萃取–同位素内标-气相色谱串联三重四极杆质谱法测定水产品中四聚乙醛残留量

Determination of metaldehyde residues in aquatic products by gas chromatography-tandem triple quadrupole mass spectrometry combined with dispersive solid phase extraction-isotope internal standard

通过优化水产品样品前处理方法,建立一种分散固相萃取-同位素内标-气相色谱串联三重四极杆质谱法测定水产品中四聚乙醛残留量方法.取5.0 g水产品,乙腈提取,PSA和C18粉净化,上清液经浓缩、正己烷定容后,采用三重四极杆串联质谱的选择多反应监测模式检测,内标法定量.研究结果表明,本方法中四聚乙醛在0.002—0.120 mg·L^(−1)范围内具有良好的线性关系,相关系数0.9999,加标回收率103.0%—114.6%,检出限0.001 mg·kg^(−1),定量限0.002 mg·kg^(−1).本方法具有操作简单、灵敏度高等特点,适用于大量水产品中四聚乙醛残留量的检测.

An analytical method was developed for the determination of metaldehyde residues in aquatic products using GC-MS/MS combined with dispersive solid phase extraction-isotope internal standard.5.0 g aquatic product samples were extracted with acetonitrile and purified with PSA and C18.After the supernatant was concentrated and redissolved with n-hexane,the supernatant was detected by tandem mass spectrometry in MRM mode and quantified by internal standard method.The method displayed good linearity in the concentration of metaldehyde ranged from 0.002 mg·L^(−1)to 0.120 mg·L^(−1)with the correlation coefficient of 0.9999,the average recoveries ranged from 103.0%to 114.6%,the limit of detection of 0.004 mg·kg^(−1)and the limit of quantification of 0.002 mg·kg^(−1).This method is fast,ensitivity and suitable for determination of metaldehyde residues in numbers of aquatic products.