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采用液相色谱-电喷雾电离质谱法对人尿液中的沙丁胺醇进行定量分析。

Quantitation of salbutamol in human urine by liquid chromatography-electrospray ionization mass spectrometry.

作者信息

Zhang Jianli, Xu Youxuan, Di Xin, Wu Moutian

机构信息

China Doping Control Center, National Research Institute of Sports Medicine, The State Sport General Administration, 1 Anding Road, Beijing 100029, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Feb 2;831(1-2):328-32. doi: 10.1016/j.jchromb.2005.11.041. Epub 2005 Dec 15.

Abstract

A sensitive and specific liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) is described for quantitation of salbutamol in human urine using nadolol as the internal standard (I.S.). Urine samples were hydrolyzed with beta-glucuronidase followed by a solid-phase extraction procedure using Bond Elut-Certify cartridges. The HPLC column was an Agilent Zorbax SB-C(18) column. A mixture of 0.01 M ammonium formate buffer (pH 3.5)-acetonitrile (85:15, v/v) was used as the mobile phase. Analytes were quantitated using positive electrospray ionization in a quadrupole spectrometer. Selected ion monitoring (SIM) mode was used to monitor m/z 166 for salbutamol and m/z 310 for I.S. Good linearity was obtained in the range of 10.0-2000.0 ng/ml. The limit of quantification was 10.0 ng/ml. The intra- and inter-run precision, calculated from quality control (QC) samples was less than 7.3%. The accuracy as determined from QC samples was within +/-2.6%. The method was applied for determining excretion curves of salbutamol.

摘要

描述了一种灵敏且特异的液相色谱 - 电喷雾电离 - 质谱法(LC - ESI - MS),以纳多洛尔作为内标(I.S.)定量测定人尿中的沙丁胺醇。尿样先用β - 葡萄糖醛酸酶水解,然后采用Bond Elut - Certify柱进行固相萃取。HPLC柱为安捷伦Zorbax SB - C(18)柱。以0.01 M甲酸铵缓冲液(pH 3.5) - 乙腈(85:15,v/v)的混合物作为流动相。在四极杆光谱仪中使用正电喷雾电离对分析物进行定量。采用选择离子监测(SIM)模式监测沙丁胺醇的m/z 166和内标的m/z 310。在10.0 - 2000.0 ng/ml范围内获得了良好的线性。定量限为10.0 ng/ml。根据质量控制(QC)样品计算的批内和批间精密度小于7.3%。由QC样品确定的准确度在±2.6%以内。该方法用于测定沙丁胺醇的排泄曲线。

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