全血中14种常见杀菌剂的实时直接分析串联质谱快速筛查研究  

Rapid Screening of 14 Common Fungicides in Whole Blood Using DART-MS/MS

作　　者：侯晓龙 吉浩城 周缘 乔静 张文芳 贾振军[1] 张瑛 HOU Xiao-long;JI Hao-cheng;ZHOU Yuan;QIAO Jing;ZHANG Wen-fang;JIA Zhen-jun;ZHANG Ying(School of Criminal Investigation,People’s Public Security University of China,Beijing 100038,China;Forensic Science Institute,Shanxi Medical University,Jinzhong 030600,China;Key Laboratory of Forensic Toxicol,Ministry of Public Security,Forensic Science Service of Beijing Public Security Bureau,Beijing 100192,China)

机构地区：[1]中国人民公安大学侦查学院,北京100038 [2]山西医科大学法医学院,山西晋中030600 [3]北京市公安司法鉴定中心法庭毒物分析公安部重点实验室,北京100192

出　　处：《分析测试学报》2025年第4期593-601,共9页Journal of Instrumental Analysis

基　　金：中国人民公安大学刑事科学技术双一流专项(2023SYL06);北京市公安局实验室专项(2023SY10006)。

摘　　要：为应对常见农药中毒案件的快速筛查,该文建立了实时直接分析串联质谱(DART-MS/MS)检测全血中14种杀菌剂的方法。通过优化质谱条件、前处理方法和DART离子源条件,确定最优方案为:用乙酸乙酯对全血样品进行液液萃取后取上清液,使用自动进样装置,取5μL样品在正离子模式、离子源温度300℃、栅极电压200 V、进样速度0.6 mm/s和离子源出口与质谱距离为1.6 cm的条件下,采用多反应监测(MRM)模式进样扫描。结果显示,14种杀菌剂的检出限为0.5~50 ng/mL,定量下限为1~100 ng/mL;平均回收率为80.8%~118%,平均基质效应为-19%~18%;定量下限以及低、高浓度质控样品的日内及日间精密度与准确度均不超过20%;除咪鲜胺、四氟咪唑、氟菌唑外,其他化合物的相关系数(r^(2))均大于0.99。该方法快速简便,满足公安检测需求。To cope with the rapid screening of common pesticide poisoning cases,a real-time direct analysis tandem mass spectrometry(DART-MS/MS)method for detecting 14 fungicides in whole blood was established.By optimizing the mass spectrometry conditions,pretreatment methods,and DART ion source conditions,the optimal scheme was determined as follows:whole blood samples were subjected to liquid-liquid extraction with ethyl acetate,and the supernatant was taken.Using an automatic sampling device,5μL of the sample was dipped and scanned in MRM mode under the conditions of positive ion mode,ion source temperature of 300℃,grid voltage of 200 V,injection speed of 0.6 mm/s,and ion source to mass spectrometry distance of 1.6 cm.The limit of detection for the 14 fungicides was 0.5-50 ng/mL,and the lower limit of quantification was 1-100 ng/mL;the average recovery was 80.8%-118%,and the average matrix effect was-19%-18%,as well as the intra-and inter-day precision and accuracy of the lower limit of quantification and the low and high concentration quality controls did not exceed 20%,and,except for prochloraz,tetrafluoroimidazole and flubacterazole,the correlation coefficients(r^(2))were all greater than 0.99.This method was fast,

关 键 词：杀菌剂 实时直接分析串联质谱(DART-MS/MS) 快速筛查 全血 

分 类 号：O657.6[理学—分析化学] Q461[理学—化学]