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[液相色谱-串联质谱法测定血清中8种有机磷农药的方法建立]

[Method establishment for the determination of 8 organophosphorus pesticides in serum using LC/MS/MS].

作者信息

Zhou Zhirong, Wang Jun, Lin Shaobin

机构信息

Institute for Environmental Health and Related Product Safety, Chinese CDC, Beijing 100021, China.

出版信息

Wei Sheng Yan Jiu. 2012 Sep;41(5):853-7.

PMID:23213707
Abstract

OBJECTIVE

To establish the method to determine the presence and concentration of 8 organophosphors pesticides in serum by LC/MS/MS.

METHOD

The serum samples were extracted by ethyl acetateether and then separated on C18 5 microm (2.1 mm x 150 mm) column with pH = 3.5 acid-ammonium acetate buffer solution, methanol--water as mobile phase to mixed gradient elution. Electro-spray ionization source (ESI) was applied and operated in positive ion mode, and multiple reaction monitoring(MRM) mode was adopted.

RESULT

Within concentration ranging from 0-1000 ng/ml the correlation coefficient for each compound was greater than 0.990, recoveries were between 95%-129%, RSD < 7.9%. The RSD of intra-day and inter-day were less 12% (n = 6).

CONCLUSION

The procedure of preparing serum samples is sample and the result of this method is efficient, accurate and specific.

摘要

目的

建立液相色谱-串联质谱法测定血清中8种有机磷农药的方法。

方法

血清样品用乙酸乙酯-乙醚萃取,然后在pH = 3.5的乙酸铵缓冲溶液、甲醇-水为流动相的C18 5微米(2.1毫米×150毫米)柱上进行分离,采用混合梯度洗脱。采用电喷雾电离源(ESI),以正离子模式运行,并采用多反应监测(MRM)模式。

结果

在0-1000纳克/毫升的浓度范围内,各化合物的相关系数均大于0.990,回收率在95%-129%之间,相对标准偏差(RSD)<7.9%。日内和日间RSD均小于12%(n = 6)。

结论

血清样品制备过程简单,该方法结果高效、准确、特异。

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