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作 者:赵海香[1,2] 郭振福[1] 汪丽萍[3] 袁光耀[1] 赵孟彬[2] 邱月明[4]
机构地区:[1]河北北方学院农林科技学院,张家口075000 [2]北京锦绣大地农业股份有限公司,北京100049 [3]国家粮食局科学研究院,北京100037 [4]中国标准化研究院,北京100088
出 处:《理化检验(化学分册)》2010年第7期820-824,828,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:北京市海淀区科委企业博士后科研专项(k2008198)
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-气相色沓质谱法(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8min。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。Methods of GC-MS(SIM) and C-C-MS/MS were applied to simultaneous determination of 6 diuretics in tea drinks with microwave assisted derivatizatiora 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 RSDfs (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%.
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