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基质辅助激光解吸电离-傅里叶变换离子回旋共振质谱法快速测定全血及尿液中的百草枯
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陈超,罗辉泰,张秋炎,杨运云,向章敏,刘舒芹 广东省科学院广东省测试分析研究所(中国广州分析测试中心)广东省原位电离质谱分析工程技术研究中心 
基金项目:广东省科学院发展专项资金项目(2020GDASYL-20200103047)
中文摘要:该文建立了一种利用基质辅助激光解吸电离-傅里叶变换离子回旋共振质谱(MALDI-FTICR-MS)快速测定全血及尿液中百草枯的分析方法。采用含1%甲酸的乙腈溶液从生物样品中提取百草枯,并与2,5-二羟基苯甲酸溶液混合后直接进样分析。结果表明,全血、尿液和水中的百草枯在10~5 000 μg/L质量浓度范围内线性良好,相关系数(r)为0.995 5~0.999 2;3种基质下的方法检出限(LOD,S/N=3)为0.6~3.0 μg/L,定量下限(LOQ,S/N=10)为2.0~10 μg/L;百草枯在全血和尿液中的平均回收率为85.2%~110%,相对标准偏差(RSD)为0.40%~7.3%。该方法具有所需样品和溶剂用量少,操作简单,分析速度快,灵敏度高,且稳定可靠等特点,可满足临床及司法鉴定相关的中毒快检需求。
中文关键词:百草枯  基质辅助激光解吸电离-傅里叶变换离子回旋共振质谱  全血  尿液
 
Rapid Determination of Paraquat in Whole Blood and Urine by Matrix Assisted Laser Desorption Ionization-Fourier Transform Ion Cyclotron Resonance Mass Spectrometry
Abstract:A matrix assisted laser desorption ionization-Fourier transform ion cyclotron resonance mass spectrometric(MALDI-FTICR-MS) method was developed for rapid determination of paraquat in whole blood and urine.The sample was extracted by liquid-liquid extraction method,with acetonitrile solution containing 1% formic acid as extraction solvent.Prior to analysis,the extracted solution was mixed with 2,5-dihydroxybenzoic acid.Results showed that there were good linear relationships for paraquat in whole blood and urine samples in the mass concentration range of 10-5 000 μg/L,with correlation coefficients(r) of 0.995 5-0.999 2.The limits of detections(LODs) and limits of quantitations(LOQs) of the method were in the ranges of 0.6-3.0 μg/L and 2.0-10 μg/L,respectively.The average recoveries at spiked levels ranged from 85.2% to 110%,with relative standard deviations(RSDs) of 0.40%-7.3%.The method showed the advantages of low sample and solvent consumption,simple operation,rapid analysis and high sensitivity,and could meet the requirements for rapid detection of clinical poisoning and forensic.
Key Words:paraquat  matrix assisted laser desorption ionization-Fourier transform ion cyclotron resonance mass spectrometry  whole blood  urine
引用本文:陈超,罗辉泰,张秋炎,杨运云,向章敏,刘舒芹.基质辅助激光解吸电离-傅里叶变换离子回旋共振质谱法快速测定全血及尿液中的百草枯[J].分析测试学报,2020,39(9):1126-1130.
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