摘要
应用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap HRMS)建立了筛查动物肌肉组织中16种新型琥珀酸脱氢酶抑制剂类杀菌剂农药残留的方法。样品使用乙腈提取,乙二胺-N-丙基硅烷(PSA)、十八烷基键合硅胶(C_(18))净化处理,数据采集使用一级母离子全扫描及数据依赖的二级子离子扫描(Full MS/dd-MS^(2))模式。以Full MS一级质谱全扫描提取母离子精确质量数所得的色谱峰面积进行定量,以保留时间和dd-MS^(2)数据依赖子离子扫描所得的二级子离子质谱图进行定性确证。结果表明,16种杀菌剂的精确质量偏差的绝对值低于4.85×10^(-6);16种杀菌剂在一定质量浓度范围内线性关系良好(R^(2)≥0.9983),方法检出限为0.12~0.60μg/kg,平均回收率为67.1%~111.9%,相对标准偏差(RSDs)为0.3%~12%。
A screening method for the rapid determination of 16 novel succinate dehydrogenase inhibitor(SDHIs)fungicide pesticide residues in animal muscle tissues was established by using high-performance liquid chromatography-quadrupole/electrostatic orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap HRMS).The samples were extracted with acetonitrile,cleaned up with ethylenediamine-N-propylsilane(PSA)and octadecyl bonded silica(C_(18)),and the data were collected using the primary precursor ion full scan and data-dependent secondary product ion scan(Full MS/dd-MS^(2))mode.The chromatographic peak areas obtained by extracting the accurate mass of the precursor ion from the Full MS primary mass spectrometry were used for quantification,and the retention time and the secondary product ion mass spectra obtained by dd-MS^(2)data-dependent product ion scanning were used for qualitative confirmation.The results showed that the absolute values of the accurate mass deviations of the 16 kinds of fungicides were lower than 4.85×10^(-6);the 16 kinds of pesticides had good linear relationships(R^(2)≥0.9983)in their respective mass concentration ranges.The detection limits(LODs)were 0.12-0.60μg/kg,the average recoveries were 67.1%-111.9%,and the relative standard deviations(RSDs)were 0.3%-12%.
作者
古飞燕
梁明
段宁馨
邹玉婷
赵晓娟
冼燕萍
GU Feiyan;LIANG Ming;DUAN Ningxin;ZOU Yuting;ZHAO Xiaojuan;XIAN Yanping(College of Light Industry and Food Science,Zhongkai University of Agriculture and Engineering,Key Laboratory of Green Processing and Intelligent Manufacturing of Lingnan Specialty Food,Ministry of Agriculture,Provincial Key Laboratory of Lingnan Specialty Food Science and Technology,Guangzhou 510225,China;Guangzhou Quality Supervision and Testing Institute,Guangzhou 511447,China)
出处
《分析试验室》
EI
CAS
CSCD
北大核心
2023年第7期944-950,共7页
Chinese Journal of Analysis Laboratory
基金
广东省岭南特色食品科学与技术重点实验室(2021B1212040013)
仲恺农业工程学院2022年研究生科技创新基金项目(KJCX2022009)资助
关键词
四极杆/静电场轨道阱高分辨质谱
农药残留
筛查
肌肉
QUECHERS
quadrupole/electrostatic field orbitrap high-resolution mass spectrometry
pesticide residues
screening
muscle
QuEChERS
作者简介
古飞燕,女(1993-),硕士研究生。研究方向:食品安全检测,15917995873@163.com;通信作者:赵晓娟,女(1980-),博士,教授。研究方向:食品安全检测,xiao0692@163.com;通信作者:冼燕萍,女(1975-),硕士,教授级高工。研究方向:食品安全研究,13642613459@139.com
