气相色谱-质谱法测定茶饮料中6种利尿剂
GC-MS Determination of 6 Diuretics in Tea Drink
摘 要
提出了同时测定茶饮料中6种利尿剂的微波辅助衍生化-气相色谱-质谱法(选择离子监测模式)[GC-MS(SIM)]和气相色谱-串联质谱(GC-MS/MS)法.样品经乙酸乙酯提取,弗罗里硅土固相萃取柱净化富集后,以碘甲烷、丙酮、碳酸钾为衍生化试剂,采用微波加热使衍生时间缩短为8 min.GC-MS(SIM)和GC-MS/MS两种方法的日内和日间相对标准偏差(n=6)均小于10%,但GC-MS/MS法的检出限(3S/N)和测定下限(10S/N)远低于GC-MS(SIM)法的数值.应用GC-MS/MS法测定茶饮料中6种利尿剂,回收率在65.1%~108.5%之间.
利尿剂
微波辅助衍生化
茶饮料
GC-MS
Diuretics
Microwave assisted derivatization
Tea drink
Abstract
Methods of GC-MS(SIM) and GC-MS/MS were applied to simultaneous determination of 6 diuretics in tea drinks with microwave assisted derivatization.The sample was extracted with ethyl acetate and purified on Florisil SPE column.Under the microwave-heating condition,the time of derivatization with CH3I,acetone and K2CO3 was shortened to 8 min.It was found that values of intraday and interday RSD′s (n=6) of the method were less than 10%.Values of detection limit (3S/N) and lower limit of determination (10S/N) by GC-MS/MS was far lower than those obtained by GC-MS(SIM).The method of GC-MS/MS was applied to the analysis of samples of tea drinks,giving values of recovery in the range of 65.1%-108.5%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 北京市海淀区科委企业博士后科研专项(k2008198)
收稿日期 2009/4/5
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备注赵海香(1969-),女,内蒙赤峰人,副教授,博士,从事农药兽药残留分析研究.
引用该论文: ZHAO Hai-xiang,GUO Zhen-fu,WANG Li-ping,YUAN Guang-yao,ZHAO Meng-bin,QIU Yue-ming. GC-MS Determination of 6 Diuretics in Tea Drink[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(7): 820～824
赵海香,郭振福,汪丽萍,袁光耀,赵孟彬,邱月明. 气相色谱-质谱法测定茶饮料中6种利尿剂[J]. 理化检验－化学分册, 2010, 46(7): 820～824
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【3】BARANOWSKA I,MARKOWSKI P,BARANOWSKI J.Simultaneous determination of 11 drugs belonging to four different groups in human urine samples by reversed-phase high-performance liquid chromatography method[J].Anal Chim Acta,2006,570:46-58．
【4】LALLJIE S P D,BARROSOB M B,STEENACKERSA D,et al.Micellar electrokinetic chromatography as a fast screening method for the determination of the doping agents furosemide and piretanide in urine[J].Journal of Chromatography B,1997,688:71-78．
【5】GUZMAN A,AGUI L,PEDRERO M,et al.Flow injection and HPLC dermination of furosemide using pulsed amperometric detection at microelectrodes[J].J Pharm Biomed Anal,2003,33:923-933．
【6】LUIS M L,FRAGA J M G,JIMNEZ,et al.Simultaneous spectrophotometric determination of diuretics by using multivariate calibration methods[J].Talanta,2001,53:761-770．
【7】朱永林,贡玉清,邵德佳,等.高效液相色谱-串联质谱法测定动物尿液中8种利尿剂残留量[J].中国兽药杂志,2008,42(9):6-12．
【8】秦旸,徐友宣,吴侔天.液相色谱-质谱法快速筛选人尿中26种利尿剂[J].质谱学报,2007,28(4):229-232．
【9】MORRA V,DAVIT P,CAPRA P,et al.Fast gas chromatographic/mass spectrometric determination diuretics and masking agents in human urine Development and validation of a productive screening protocol for antidoping analysis[J].Journal of Chromatography A,2006,1135:219-229．
【10】BARROSO M B,MEIRING H D,JONG A,et al.Gas chromatographic-mass spectrometric analysis of the loop diuretic torasemide in human urine[J].Journal of Chromatography B,1997,690:105-113．
【11】SEGURA J,VENTURA R,JURADO C.Review derivatization procedures for gas chromatographicy-mas spectrometric determination of xenobiotics in biological samples,with special attention to drugs of abuse and doping agents[J].Journal of Chromatography B,1998,713:61-90．
【12】AMENDOLA L,COLAMONICI C,MAZZARINO M,et al.Rapid determination of diuretics in human urine by gas chromatography-mass spectrometry follow in microwave assisted derivatization[J].Anal Chim Acta,2003,475:125-136．
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