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,1.8μm)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0.1～500.0μg/L范围内线性良好(R2>0.997);检出限介于0.02～0.3μg/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。
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（R20.997） 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.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2012年第12期1852-1858,共7页
Chinese Journal of Analytical Chemistry
基金
"十二五"国家科技支撑计划(No.2011BAK10B07)资助项目
关键词
单端孢霉烯族毒素
代谢物
固相萃取
液质联用
血浆
T-2 toxin
Metabolites
Solid phase extraction
Ultra performance liquid chromatography tandem mass spectrometry
Plasma
