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10~5000μg/L质量浓度范围内线性良好,相关系数(r)为0.9955~0.9992;3种基质下的方法检出限(LOD,S/N=3)为0.6~3.0μg/L,定量下限(LOQ,S/N=10)为2.0~10μg/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。
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 10-5000μg/L,with correlation coefficients(r)of 0.9955-0.9992.The limits of detections(LODs)and limits of quantitations(LOQs)of the method were in the ranges of 0.6-3.0μg/L and 2.0-10μg/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.
作者
陈超
罗辉泰
张秋炎
杨运云
向章敏
刘舒芹
CHEN Chao;LUO Hui-tai;ZHANG Qiu-yan;YANG Yun-yun;XIANG Zhang-min;LIU Shu-qin(Guangdong Provincial Engineering Research Center for Ambient Mass Spectrometry,Guangdong Institute of Analysis(China National Analytical Center Guangzhou),Guangdong Academy of Sciences,Guangzhou 510070,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2020年第9期1126-1130,共5页
Journal of Instrumental Analysis
基金
广东省科学院发展专项资金项目(2020GDASYL-20200103047)。
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
paraquat
matrix assisted laser desorption ionization-Fourier transform ion cyclotron resonance mass spectrometry
whole blood
urine
