超高效液相色谱-大气压化学电离-串联质谱法快速测定禽蛋中地克珠利和妥曲珠利残留标识物  

Fast Determination of Diclazuril and Toltrazuril Residue Makers in Eggs by Ultra-high Performance Liquid Chromatography-Atmospheric Pressure Chemical Ionization-Triple Quadrupole Mass Spectrometry

作　　者：张海超 魏欣欣 张婧雯 贾海涛 艾连峰 王敬 黄雪静 秦晓航 刘宝如 ZHANG Haichao;WEI Xinxin;ZHANG Jingwen;JIA Haitao;AI Lianfeng;WANG Jing;HUANG Xuejing;QIN Xiaohang;LIU Baoru(Shijiazhuang Customs Technology Center,Shijiazhuang 050051,China)

机构地区：[1]石家庄海关技术中心,河北石家庄050051

出　　处：《食品科学》2025年第8期330-335,共6页Food Science

基　　金：河北省科技计划项目(21475501D)。

摘　　要：建立超高效液相色谱-大气压化学电离-串联质谱法快速分析禽蛋中地克珠利和妥曲珠利残留标识物的分析方法。本实验采用乙腈提取目标化合物,经通过式固相萃取柱净化,采用ACQUITY BEH C18色谱柱(2.1 mm×100 mm,1.7μm)分离,乙腈-0.1%甲酸水进行梯度洗脱,采用大气压化学电离源电离,在负离子多反应监测扫描模式下测定,内标法定量。地克珠利和妥曲珠利砜在0.5~200 ng/mL线性范围内呈良好线性关系,决定系数大于0.9990,检出限为0.5μg/kg,定量限为2μg/kg。待测物平均回收率在72.8%~106.5%之间,相对标准偏差在3.2%~8.5%之间。该方法简单、准确、灵敏度高,可用于禽蛋中地克珠利、妥曲珠利残留量的快速检测与确证。A comprehensive analytical method was developed for the determination of diclazuril and toltrazuril residue makers in eggs by ultra-high performance liquid chromatography-atmospheric pressure chemical ionization-triple quadrupole mass spectrometry(UPLC-APCI-MS/MS).Samples were extracted with acetonitrile and purified using a PRiME hydrophilic-lipophilic balance(HLB)column.Chromatographic separation was achieved on a ACQUITY BEH C18 column(2.1 mm×100 mm,1.7μm)by gradient elution with a mobile phase composed of acetonitrile and 0.1%formic acid solution.An APCI interface was used as the ion source and the analysis was performed using negative ionization in multiple reaction monitoring(MRM)mode.An internal standard calibration curve method was employed for quantification.The calibration curves were linear in the range of 0.5–200 ng/mL with determination coefficients of more than 0.9990.The limits of detection(LODs)were 0.5μg/kg,and the limits of quantization(LOQs)were 2μg/kg.The average recoveries of the analytes range from 72.8%to 106.5%,with relative standard deviations(RSDs)of 3.2%–8.5%.The developed method is simple,accurate,sensitive,and useful for the rapid detection and confirmation of diclazuride and toltrazuril sulfone residues in eggs.

关 键 词：超高效液相色谱-三重四极杆质谱 大气压化学电离 禽蛋 地克珠利 妥曲珠利砜 

分 类 号：O657.63[理学—分析化学]