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	超高效液相色谱- 串联质谱同时检测血液中29种农药
其他题名	Detection of 29 pesticides in the blood by ultra high performance liquid chromatography-series mass spectrometry
	白利文; 王瑞花; 于忠山; 钟世豪; 于哲
来源期刊	化学研究与应用
ISSN	1004-1656
出版年	2020
卷号	32 期号:1 页码:150-156
中文摘要	本文采用超高效液相色谱-串联质谱法( UPLC-MS /MS)和固相萃取法( SPE)建立了血液中29种农药同时筛查、定性、定量分析的方法,血液经4%磷酸水溶液稀释后,震荡10min,以8000r·min~(-1)转速离心 10min,取上清液过3mL甲醇和3mL水活化好的Oasis Prime HLB( 3cc,60mg)固相萃取小柱,使用3mL5%甲醇水淋洗,3 mL乙腈甲醇混合溶剂( 90: 10)洗脱,接收洗脱液后在40℃条件下氮吹仪吹干,使用0. 5mL初始流动相复溶,震荡10s后,过0. 22mum水膜,装液质小瓶后进样分析。采用ACQUITY UPLC HSS C18色谱柱( 150 mm* 2. 1mm, 1. 8mum)分离,流动相为0. 1%甲酸乙腈-水/甲酸/甲酸铵( 5mmol,pH= 3) ,梯度洗脱,电喷雾电离正离子模式( ESI+) ,多反应选择离子监测模式( MRM)检测。29种农药的检出限为0. 1 ng·mL~(-1) ~ 5 ng·mL~(-1),定量限为0. 5 ng·mL~(-1) ~ 10 ng·mL~(-1),回收率为62. 4%~ 97. 4%,基质效应为82. 8%~ 109%,相对标准偏差小于10. 3%,相关系数均大于0. 99,线性关系良好范围为10 ng·mL~(-1) ~ 1000ng·mL~(-1)。本文方法灵敏度高,可以对血液中29种农药成分进行筛查、定性、定量分析,能够满足实际血液样品中农药成分检测的需求。
英文摘要	In this paper,ultra-high performance liquid chromatography-tandem mass spectrometry( UPLC-MS /MS) and solid phase extraction( SPE) were used to establish a method for simultaneous screening,qualitative and quantitative analysis of 29 pesticides in blood.After the blood was diluted with 4%phosphoric acid solution, shaken for 10 min, centrifuged at 8000 r·min~(-1) for 10 min.Oasis Prime HLB( 3 cc, 60 mg) solid phase extraction cartridge was activated with 3 mL methanol and 3 mL water, then the supernatant was taken through a solid phase extraction cartridge.Rinse the solid phase extraction cartridge with 3 mL 5%methanol water, and elute the target compound using 3 mL mixed solvent of acetonitrile and methanol( 90 ∶ 10) . After receiving the eluent, it was dried by nitrogen at 40 ° C, reconstituted with 0. 5 mL initial mobile phase, shaken for 10 s, and passed through a 0. 22 mum water film.The filtrate was loaded into a vial dedicated to liquid chromatography and mass spectrometry,and the sample was analyzed.The target compound was separated using an ACQUITY UPLC HSS C18 column( 150 mm * 2. 1 mm, 1. 8 mum) . The mobile phase used 0. 1% formic acid acetonitrile-water /formic acid /ammonium formate( 5 mmol,pH= 3) . Set the mobile phase gradient to elute and separate the target compound.Electrospray ionization,positive ion mode( ESI+ ) , and monitor target compounds in multiple reaction selective ion monitoring mode( MRM) . The detection limit of 29 pesticides was 0. 1 ng·mL~(-1) ~ 5 ng·mL~(-1) .The limit of quantification was 0. 5 ng·mL~(-1) ~ 10 ng·mL~(-1) .The recovery was 62. 4%~ 97. 4%, and the matrix effect was 82. 8%~ 109%. The standard deviation was less than 10. 3%. The correlation coefficient was greater than 0. 99, and the linear relationship was in the range of 10 ng·mL~(-1) ~ 1000 ng·mL~(-1) .The method has high sensitivity and can screen,qualitatively and quantitatively analyze 29 pesticide components in blood,which can meet the requirements of pesticide component detection in actual blood samples.
中文关键词	液相色谱-串联质谱 ; 检测 ; 农药 ; 血液 ; 固相萃取
英文关键词	UPLC-MS /MS screening pesticides blood SPE
类型	Article
语种	中文
收录类别	CSCD
WOS类目	Chemistry
CSCD记录号	CSCD:6666609
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/353613
作者单位	白利文, 中国人民公安大学刑事科学技术专业, 北京 100038, 中国. 钟世豪, 中国人民公安大学刑事科学技术专业, 北京 100038, 中国. 于哲, 中国人民公安大学刑事科学技术专业, 北京 100038, 中国. 王瑞花, 公安部物证鉴定中心, 北京 100038, 中国. 于忠山, 公安部物证鉴定中心, 北京 100038, 中国.
推荐引用方式 GB/T 7714	白利文,王瑞花,于忠山,等. 超高效液相色谱- 串联质谱同时检测血液中29种农药[J],2020,32(1):150-156.
APA	白利文,王瑞花,于忠山,钟世豪,&于哲.(2020).超高效液相色谱- 串联质谱同时检测血液中29种农药.化学研究与应用,32(1),150-156.
MLA	白利文,et al."超高效液相色谱- 串联质谱同时检测血液中29种农药".化学研究与应用 32.1(2020):150-156.