固相萃取-超高效液相色谱-质谱联用技术检测大鼠血浆中T-2毒素及其主要代谢产物

引用本文: 赵燕华, 林妮妮, 郭磊, 陈佳, 刘万卉, 谢剑炜. 固相萃取-超高效液相色谱-质谱联用技术检测大鼠血浆中T-2毒素及其主要代谢产物[J]. 分析化学, 2012, 40(12): 1852-1858. doi: 10.3724/SP.J.1096.2012.20124 shu

Citation: ZHAO Yan-Hua, LIN Ni-Ni, GUO Lei, CHEN Jia, LIU Wan-Hui, XIE Jian-Wei. Simultaneous Determination of T-2 Toxin and Its Metabolites in Rat Plasma Using Solid Phase Extraction and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2012, 40(12): 1852-1858. doi: 10.3724/SP.J.1096.2012.20124 shu

固相萃取-超高效液相色谱-质谱联用技术检测大鼠血浆中T-2毒素及其主要代谢产物

赵燕华 ^1,2, ,
林妮妮 ^1, ,
郭磊 ^1, ,
陈佳 ^1, ,
刘万卉 ^2, ,
谢剑炜 ^{1,
,}

通讯作者: 谢剑炜

基金项目:
本文系"十二五"国家科技支撑计划(No.2011BAK10B07)资助项目 (No.2011BAK10B07)

摘要: 应用固相萃取-超高效液相色谱-三重四极杆-线性离子阱串联质谱技术,建立了高灵敏度的大鼠血浆中单端孢霉烯族(T-2)毒素及其5种主要代谢物的分析方法。在优化的固相萃取条件下,大鼠血浆经HLB固相萃取柱净化富集后,以XDB-C₁₈色谱柱(50 mm×4.6 mm,1.8 μm)分离,以5 mmol/L乙酸铵溶液和甲醇溶液为流动相进行梯度洗脱,以玉米赤霉酮为内标,在正离子多反应监测模式下对各分析物进行定性和定量分析。各分析物在0.1-500.0 μg/L范围内线性良好(R²>0.997);检出限介于0.02-0.3 μg/L之间;加标回收率为93.5%-120.3%;相对标准偏差均小于13%。本方法快速、重现性好、灵敏度高,已成功应用于T-2毒素中毒的溯源性研究。

关键词:

English

Simultaneous Determination of T-2 Toxin and Its Metabolites in Rat Plasma Using Solid Phase Extraction and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

1.
¹ College of Pharmacy, Yantai University, Yantai 264005, China;

Corresponding author: 谢剑炜

Received Date: 15 March 2012
Fund Project:
本文系"十二五"国家科技支撑计划(No.2011BAK10B07)资助项目

Abstract: T-2 toxin and its 5 metabolites in rat plasma were simultaneously determined by an ultra performance liquid chromatography coupled with triple quadrupole-ion trap mass spectrometric (UPLC-QTRAP) method with high sensitivity. In the optimized solid phase extraction conditions, the rat plasma samples were purified and concentrated by a HLB column, and then the analytes were separated on a XDB-C18 column (4.6 mm×50 mm, 1.8 μm) with a mobile phase of methanol and aqueous solution containing 5 mmol/L ammonium acetate under a gradient elution. The mass spectrometric identification and quantification were performed with electrospray ionization in a positive by using multiple reaction monitoring mode with zearalanone as internal standard. In this established method, good linearities (R²>0.997) in the range from 0.1 to 500 μg/L with the limits of detection between 0.02 to 0.3 μg/L, and the recoveries varied from 93.5% to 120.3% with a relative standard deviations less than 13% were obtained. The method is rapid, reproducible, sensitive, and can be applied in the retrospective determination of the intoxication event of T-2 toxin.

Key words:

T-2 toxin
/ Metabolites
/ Solid phase extraction
/ Ultra performance liquid chromatography tandem mass spectrometry
/ Plasma

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

固相萃取-超高效液相色谱-质谱联用技术检测大鼠血浆中T-2毒素及其主要代谢产物

通讯作者: 谢剑炜

English

Simultaneous Determination of T-2 Toxin and Its Metabolites in Rat Plasma Using Solid Phase Extraction and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: 谢剑炜

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

固相萃取-超高效液相色谱-质谱联用技术检测大鼠血浆中T-2毒素及其主要代谢产物

通讯作者: 谢剑炜

English

Simultaneous Determination of T-2 Toxin and Its Metabolites in Rat Plasma Using Solid Phase Extraction and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: 谢剑炜

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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