液相色谱-质谱法测定兔泪液中的甲砜霉素
Liquid chromatography-mass spectrometry method for the determination of thiamphenicol in rabbit tears.
作者信息
Tian Dafeng, Feng Feng, Li Ying, Yang Jianhong, Tian Xiaolin, Mo Fengkui
机构信息
Department of Pharmacy, School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, PR China.
出版信息
J Pharm Biomed Anal. 2008 Nov 4;48(3):1015-9. doi: 10.1016/j.jpba.2008.07.002. Epub 2008 Jul 11.
A simple and sensitive liquid chromatography-mass spectrometry (LC-MS) method was described for the determination of thiamphenicol in rabbit tears. Chromatographic separation of the analyte was achieved on a C18 column using a mobile phase of acetonitrile and 10 mmol/l ammonium acetate solution (60:40, v/v). Selected ion monitoring (SIM) in negative mode was used for analyte quantification at m/z 354.4 for thiamphenicol and at m/z 137.1 for salylic acid. The run time was less than 6 min. Linearity over the concentration range of 0.032-32.0 ng/ml for thiamphenicol was obtained and the lower limit of quantification was 0.032 ng/ml. For each level of QC samples, inter- and intra-day precisions (R.S.D.) were <or=5.2% and 8.3%, respectively, and the accuracy (RE) was +/-2.8%. The present LC-MS method was successfully applied to the pharmacokinetic studies of thiamphenicol in situ forming gel in rabbit tears.
描述了一种简单且灵敏的液相色谱 - 质谱（LC - MS）方法，用于测定兔泪液中的甲砜霉素。在C18柱上，以乙腈和10 mmol/L醋酸铵溶液（60:40，v/v）作为流动相实现了分析物的色谱分离。采用负模式下的选择离子监测（SIM）对分析物进行定量，甲砜霉素在m/z 354.4处，水杨酸在m/z 137.1处。运行时间少于6分钟。甲砜霉素在0.032 - 32.0 ng/ml浓度范围内具有线性，定量下限为0.032 ng/ml。对于每个质量控制样品水平，日内和日间精密度（相对标准偏差，R.S.D.）分别≤5.2%和8.3%，准确度（相对误差，RE）为±2.8%。本LC - MS方法成功应用于甲砜霉素原位形成凝胶在兔泪液中的药代动力学研究。
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