微管纸喷雾质谱法快速筛查血液中5种强极性毒物  

Fast Screening of 5 Polar Poisons in Blood Sample by Paper Capil⁃lary Spray Tandem Mass Spectrometry

作　　者：张云峰[1] 董林沛 赵森[2] 孙龙 常靖[1] 任昕昕[1] 王爱华[1] ZHANG Yun-feng;DONG Lin-pei;ZHAO Sen;SUN Long;CHANG Jing;REN Xin-xin;WANG Ai-hua(Institute of Forensic Science,Ministry of Public Security,Beijing 100038,China;Zhejiang Police College,Hangzhou 310053,China;PURSPEC Technologies,Beijing 100084,China)

机构地区：[1]公安部物证鉴定中心,北京100038 [2]浙江警察学院,浙江杭州310053 [3]北京清谱科技有限公司,北京100084

出　　处：《分析测试学报》2022年第4期652-658,共7页Journal of Instrumental Analysis

基　　金：“十三五”国家重点研发计划(25903)。

摘　　要：采用微管纸喷雾质谱法快速筛查了血液中的敌草快、百草枯、草甘膦、草铵膦和氯化琥珀胆碱5种强极性毒物。全血样品用9倍样品体积的甲醇提取,静置后取上清液直接上样,使用多反应监测扫描模式,每个化合物测定两个离子进行定性和定量分析。5种极性物质可在1 min内完成检测。该方法对5种极性毒物的检出限分别为敌草快0.05 mg/L,百草枯0.5 mg/L,草甘膦25 mg/L,草铵膦25 mg/L,氯化琥珀胆碱0.05 mg/L。敌草快和氯化琥珀胆碱的线性范围为0.005~0.5 mg/L,百草枯的线性范围为0.05~5 mg/L,草甘膦和草铵膦的线性范围为2.5~100 mg/L,可满足快速筛查检测的使用需求。样品在1倍、2倍和10倍检出限加标浓度下的回收率为62%~117%,相对标准偏差不大于40%。该方法操作简便、高效快速,适用于全血样品中上述5种极性毒物的快速筛查。A fast screening method was developed for the analysis of five extremely polar poisons in whole blood sample using paper capillary spray(PCS)tandem mass spectrometry.The five extremely polar poisons are diquat,paraquat,glyphosate,glufosinate-ammonium and succinylcholine chlo⁃ride.The whole blood sample was extracted with methanol,at a ratio of 1 to 9(by volume)for sam⁃ple and methanol.After mixing the sample and keeping it static,100μL supernatant was loaded on⁃to the paper capillary spray cartridge.The cartridge was then inserted into the inlet of PURSPEC MS Mate interface,which was coupled to a Shimadzu 8040 tandem mass spectrometry system.After⁃wards,the analytes were directly analyzed qualitatively and quantitatively using the two precursor ion-product ion pairs with multiple reaction monitoring(MRM)mode.With the help of no complicat⁃ed sample preparation provided by PCS cartridge as an ambient ionization technique,together with the direct coupling of PCS to commercial instrument by MS Mate,the five polar targets could be de⁃tected within 1 minute,which is much faster than current methods.During the research process,the mass spectrometry parameters were optimized first,and the ion pairs for each analyte were found with their corresponding standard solutions.The qualitative and quantitative ion pairs are listed as follows:diquat(positive mode,183.1>157.0*,183.1>130.0),paraquat(positive mode,185.1>170.1,186.1>171.1*),glyphosate(negative mode,168.0>63.0,168.0>150.0*),glufosinate-ammonium(negative mode,180.1>85.0*,180.1>136.0),and succinylcholine chloride(positive mode,145.1>93.6,145.1>115.5*),where the ion pairs with the asterisk re⁃fer to quantitative ion pairs.The limits of detection(LODs)for the five polar compounds in blood sam⁃ple were 0.05 mg/L for diquat,0.5 mg/L for paraquat,25 mg/L for glyphosate,25 mg/L for glufos⁃inate-ammonium,and 0.05 mg/L for succinylcholine chloride.Here the definition of signal-to-noise(S/N)ratio no less than 3 was used for LOD measurement.Linearity was measure

关 键 词：微管纸喷雾 原位电离 极性物质 全血样品 

分 类 号：O657.63[理学—分析化学] R991[理学—化学]