文章摘要
陈安九,李 浩,王源园,孙鲁宁,唐 茜,张宏文,方云茜,王永庆.LC-MS/MS法测定人尿液中索法酮的浓度及其尿药排泄研究[J].南京医科大学学报,2014,(5):676~679
LC-MS/MS法测定人尿液中索法酮的浓度及其尿药排泄研究
Determination of sofalcone by LC-MS/MS in human urine and its application to kinetic study of urinary excretion
投稿时间:2013-07-29  
DOI:10.7655/NYDXBNS20140530
中文关键词: 索法酮  LC-MS/MS  尿药排泄
英文关键词: sofalcone  LC-MS/MS  urinary excretion
基金项目:国家自然科学基金面上项目(81273593);江苏省卫生厅面上项目(H201108);南京市科技发展计划基金资助(2011YX001)
作者单位
陈安九 南京医科大学第一附属医院临床药理研究室,江苏 南京 210029 
李 浩 南京医科大学第一附属医院临床药理研究室,江苏 南京 210029 
王源园 南京医科大学第一附属医院临床药理研究室,江苏 南京 210029 
孙鲁宁 南京医科大学第一附属医院临床药理研究室,江苏 南京 210029 
唐 茜 南京医科大学第一附属医院临床药理研究室,江苏 南京 210029 
张宏文 南京医科大学第一附属医院临床药理研究室,江苏 南京 210029 
方云茜 南京医科大学第一附属医院临床药理研究室,江苏 南京 210029 
王永庆 南京医科大学第一附属医院临床药理研究室,江苏 南京 210029 
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中文摘要:
      目的:建立测定人尿液中索法酮浓度的LC-MS/MS方法,用于研究健康受试者口服索法酮后药物在体内的尿药排泄特征?方法:尿液经甲醇处理后,进行LC-MS/MS分析?色谱柱为Poroshell 120 SB-C18柱,柱温为30℃?流动相为甲醇∶2 mmol/L 醋酸铵(85∶15),流速为0.20 ml/min?负离子模式下使用电喷雾离子化和多反应离子监测?2名健康志愿者单次口服索法酮胶囊200 mg后,测定尿药浓度并研究尿药排泄特征?结果:索法酮的最低定量限为1 ng/ml,在1~500 ng/ml范围内线性关系良好,高中低3个浓度的批内?批间差均小于6%,基质效应在93.1%~114.8%范围内,提取回收率为84.7%~93.6%?尿液中索法酮的累积排泄率小于0.01%?结论:所建立的LC-MS/MS分析方法能快速?准确地测定尿液中索法酮的浓度?
英文摘要:
      Objective:To develop an LC-MS/MS method for determination of sofalcone in urine samples,and to investigate its urinary excretion characteristics in healthy Chinese volunteers. Methods:The urine samples were treated with methanol and separated on a Poroshell 120 SB-C18 column,with a mobile phase of methanol and 2 mmol/L Ammonium acetate(85∶15,v/v). The rate was 0.20 mL/min and the temperature was 30℃. Electrospray ionization source was applied and operated in the negative ion mode using SRM. Two healthy Chinese volunteers were given single oral dose of sofalcone capsule(200 mg) for urinary excretion and characteristics. Results:The lower limits of quantitation for sofalcone were 1 ng/mL,and the linear range was 1~500 ng/mL. The data of intra and inter-run precision were all less than 6%. The matrix effects were between 93.1% and 114.8%. The extraction recovery was 84.7%~93.6%. The accumulated excretion rates of sofalcone in urine were lower than 0.01%. Conclusion:The developed method can be applied to evaluate the urinary excretion of the sofalcone with a very short running time.
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