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血浆和尿液中百草枯和敌草快测定的固相萃取-液相色谱-串联质谱法
其他题名Liquid chromatography-tandem mass spectrometry method for the determination of paraquat and diquat in plasma and urine
郭翔; 李添娣; 田东超; 马常虹; 林怡然; 贠建培
来源期刊中华劳动卫生职业病杂志
ISSN1001-9391
出版年2021
卷号39期号:8页码:612-616
中文摘要目的建立血浆和尿液中百草枯和敌草快的液相色谱-串联质谱(LC-MS/MS)检测方法。方法血浆经乙腈沉淀蛋白磷酸盐缓冲液(pH=7)稀释,尿样用磷酸盐缓冲液(pH=7)直接稀释,稀释后的样品经Oasis WCX固相萃取柱萃取。以100 mmol/L甲酸铵+0.5%甲酸水溶液和乙腈为流动相,经HILIC色谱柱分离,LC-MS/MS多反应监测模式检测,百草枯内标法定量,敌草快外标法定量:结果百草枯和敌草快同在10.0~120.0g/L质量浓度范围内线性良好,相关系数为0.998 5~0.999 4。百草枯在血浆和尿液中最低检出限分别为1.98 g/L和1.00 g/L,样品加标回收率在100.2%~107.3%,相对标准偏差在1.6%~3.3%。敌草快在血浆和尿液中最低检出限分别为1.80g/L和2.77g/L,样品加标回收率在85.3%~93.1%,相对标准偏差在1.8%~5.5%。结论本方法灵敏准确,能够对血浆和尿液中的百草枯和敌草快同时进行测定。
英文摘要Objective To establish a LC-MS/MS method for determination of paraquat and diquat in plasma and urine samples.Methods Plasma is precipitated by acetonitrile then diluent with phosphate buffer (pH=7),urine is diluent with phosphate buffer(pH=7),then diluent samples extracted with Oasis WCX solid-phase extraction column.Samples were analyzed using LC-MS/MS in multiple reaction monitoring (MRM) mode.The analytical column was XBridge BEH-HILIC (100 mm*2.1 mm*2.5 m) and the mobile phase were 100 mmol ammonium formate add 0.5% formic acid and acetonitrile.Paraquat was quantified by internal standard method and diquat by external standard method.Results The calibration curves of paraquat and diquat were linear in the concentration range of 10.0~120.0 g/L,the correlation coefficient (r) were 0.9985~0.9994.The limit of detection of paraquat in plasma and urine were 1.98 g/L and 1.00 g/L,respectively,the recovery rate were 100.2%~107.3%,the RSD were 1.6%~3.3%.The limit of detection of diquat in plasma and urine were 1.80 g/L and 2.77 g/L,respectively,the recovery rate were 85.3%~93.1%,the RSD were 1.8%~ 5.5%.Conclusion This method is sensitive and accurate,and can simultaneously determine paraquat and diquat in plasma and urine.
中文关键词百草枯 ; 敌草快 ; 液相色谱-质谱 ; 血浆 ; 尿液
英文关键词Paraquat Diquat LC-MS/MS Plasma Urine
类型Article
语种中文
收录类别CSCD
WOS类目General & Internal Medicine
CSCD记录号CSCD:7040558
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/378157
作者单位郭翔, 深圳市职业病防治院, 深圳, 广东 518020, 中国.; 李添娣, 深圳市职业病防治院, 深圳, 广东 518020, 中国.; 田东超, 深圳市职业病防治院, 深圳, 广东 518020, 中国.; 马常虹, 深圳市职业病防治院, 深圳, 广东 518020, 中国.; 林怡然, 深圳市职业病防治院, 深圳, 广东 518020, 中国.; 贠建培, 深圳市职业病防治院, 深圳, 广东 518020, 中国.
推荐引用方式
GB/T 7714
郭翔,李添娣,田东超,等. 血浆和尿液中百草枯和敌草快测定的固相萃取-液相色谱-串联质谱法[J],2021,39(8):612-616.
APA 郭翔,李添娣,田东超,马常虹,林怡然,&贠建培.(2021).血浆和尿液中百草枯和敌草快测定的固相萃取-液相色谱-串联质谱法.中华劳动卫生职业病杂志,39(8),612-616.
MLA 郭翔,et al."血浆和尿液中百草枯和敌草快测定的固相萃取-液相色谱-串联质谱法".中华劳动卫生职业病杂志 39.8(2021):612-616.
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