Nishikawa M, Tsuchihashi H, Miki A, Katagi M, Schmitt G, Zimmer H, Keller T, Aderjan R
Forensic Science Laboratory, Osaka Prefectural Police Headquarters, Japan.
J Chromatogr B Biomed Sci Appl. 1999 Apr 16;726(1-2):105-10. doi: 10.1016/s0378-4347(99)00008-0.
A rapid and sensitive determination procedure using liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) has been developed for the determination of ethyl glucuronide (EtG) in human serum. Samples were precipitated with methanol, centrifuged and the supernatant was evaporated to dryness followed by reconstitution with distilled water. As mobile phase 30 mM ammonium acetate-acetonitrile (30:70, v/v) was utilized. The base peak observed at m/z 221 was the [M-H]- ion of EtG, which was detectable in satisfactory sense. The detection limit was 0.03 microg/ml in the selected ion monitoring mode. A calibration graph constructed for EtG in serum gave good linearity over the range from 0.1 to 25 microg/ml. This paper also presents the application of this LC-ESI-MS procedure to the analysis of authentic serum samples.
已开发出一种使用液相色谱 - 电喷雾电离质谱法(LC - ESI - MS)快速灵敏地测定人血清中葡萄糖醛酸乙酯(EtG)的方法。样品用甲醇沉淀,离心,上清液蒸发至干,然后用蒸馏水复溶。使用30 mM醋酸铵 - 乙腈(30:70,v/v)作为流动相。在m/z 221处观察到的基峰是EtG的[M - H]-离子,其检测效果令人满意。在选择离子监测模式下,检测限为0.03微克/毫升。血清中EtG的校准曲线在0.1至25微克/毫升范围内具有良好的线性。本文还介绍了这种LC - ESI - MS方法在真实血清样品分析中的应用。