| 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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| 基金项目:广东省科学院发展专项资金项目(2020GDASYL-20200103047) |
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| 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 |
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| Rapid Determination of Paraquat in Whole Blood and Urine by Matrix Assisted Laser Desorption Ionization-Fourier Transform Ion Cyclotron Resonance Mass Spectrometry |
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| 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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