•  
  •  
  •  
  •  
  •  
  •  
  •  
  •  
  •  
期刊检索


检索
检索项:
检索词:
总目录
  • WCSB9︱2019(第九届)世界采样和混样大会 查看全文>>
  • 关于召开第十五届全国青年分析测试学术报告会的通知 查看全文>>
友情链接
微管纸喷雾质谱法快速筛查血液中5种强极性毒物
    点此下载全文
作者单位
张云峰,董林沛,赵森,孙龙,常靖,任昕昕,王爱华 1. 公安部物证鉴定中心北京 1000382. 浙江警察学院浙江 杭州 3100533. 北京清谱科技有限公司北京 100084 
基金项目:“十三五”国家重点研发计划(25903)
中文摘要: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。
中文关键词:微管纸喷雾  ?原位电离  ?极性物质  ?全血样品
 
Fast Screening of 5 Polar Poisons in Blood Sample by Paper Capillary Spray Tandem Mass Spectrometry
Abstract: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 chloride.The whole blood sample was extracted with methanol,at a ratio of 1 to 9(by volume) for sample and methanol.After mixing the sample and keeping it static,100 μL supernatant was loaded onto 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.Afterwards,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 complicated 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 detected 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 refer to quantitative ion pairs. The limits of detection(LODs) for the five polar compounds in blood sample were 0.05 mg/L for diquat,0.5 mg/L for paraquat,25 mg/L for glyphosate,25 mg/L for glufosinate-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 measured by spiking analyte standards to the methanol extracted supernatant from blank blood sample.Good linearity was achieved in the range of 0.005-0.5 mg/L for diquat and succinylcholine chloride,in the range of 0.05-5 mg/L for paraguat,and in the range of 2.5-100 mg/L for glyphosate and glufosinate-ammonium.The spiked recovery ranged from 62% to 117% with relative standard deviation less than 40% under 1,2,10 times detection limit.Using the method developed in this article,whole blood samples from poisoned patients were analyzed and the corresponding poisons were correctly identified and quantified,which shows that the performance of the PCS-MS Mate-MS/MS method meets the need in real life for fast screening analysis.The method is convenient and suitable for the fast screening of polar poisons in blood samples.
Key Words:paper capillary spray  ?ambient ionization  ?polar compounds  ?blood sample
引用本文:张云峰,董林沛,赵森,孙龙,常靖,任昕昕,王爱华.微管纸喷雾质谱法快速筛查血液中5种强极性毒物[J].分析测试学报,2022,41(4):652-658.
摘要点击次数: 111
全文下载次数: 173
查看全文  下载PDF阅读器