在线固相萃取-二维液相色谱串联质谱法测定人脑脊液中替考拉宁浓度  

Determination of Teicoplanin in Human Cerebrospinal Fluid Using an On-line Solid Phase Extraction-Two Dimensional Liquid Chromatography-Tandem Mass Spactrometry

作　　者：左利民[1] 姚静[2] 王强[3] 周洁[1] 冯梦雪[1] 山广志[1] 

机构地区：[1]中国医学科学院医药生物技术研究所,北京100050 [2]中国食品药品检定研究院,北京100050 [3]首都医科大学附属天坛医院,北京100050

出　　处：《分析化学》2014年第12期1773-1778,共6页Chinese Journal of Analytical Chemistry

基　　金：科技部新药创制重大专项平台资助项目(No.2012zx09301002-001-019)

摘　　要：建立测定人脑脊液中替考拉宁浓度的在线固相萃取-二维液相色谱-串联质谱（ SPE-2DLC-MS/MS）法。脑脊液样品经在线固相萃取处理后,通过阀切换二维色谱技术,转载至Shiseido CAPCALL-PAK C18分析柱上进行分离,以25mmol/L乙酸铵（pH 6.0）-乙腈为流动相梯度洗脱,流速1.0 mL/min。采用电喷雾离子源（ ESI）,以选择反应监测（ SRM）方式进行正离子检测,采用氢溴酸东莨菪碱为内标,对脑脊液样本中替考拉宁浓度进行定量检测。本方法中替考拉宁浓度在25～5000μg/L的范围内线性关系良好（R2=0.9993,n=6）；日间和日内精密度RSD均小于6％,低中高3个浓度的回收率在100.8％～109.9％之间。结果表明,本方法的选择性好,线性、精密度、准确度和灵敏度高,可用于临床监测替考拉宁浓度。A method of on-line solid phase extraction （ SPE ）-two dimensional liquid chromatography electrospary-tandem mass spectrometric method was established for the determination of Teicoplanin concentrations in human cerebrospinal fluid. Cerebrospinal fluid samples were treated by the on-line SPE treatment, and analyzed by LC-MS/MS. The chromatographic separation was performed on a Shiseido CAPCALL-PAK C18 column with gradient elution by using 25 mmol/L ammonium acetate （ pH 6. 0 ）-acetonitrile as mobile phases, and the flow rate of 1 mL/min. Detection was carried out under the selected reaction monitoring （ SRM） in positive ionization mode with scopolamine hydrobromide as internal standard. Matrix-matched calibration curves with good correlation coefficients （R2=0. 9993, n=6） were obtained in the concentration range of 25-5000 μg/L. The average recoveries varied from 100. 8% to 109.9%. The intra-and inter-day precisions were less than 6%. The method is proved to be rapid, sensitive, accurate, and suitable to determine Teicoplanin concentrations in human cerebrospinal fluid.

关 键 词：在线固相萃取 替考拉宁 人脑脊液 二维液相色谱-串联质谱 

分 类 号：R969[医药卫生—药理学] O657.63[医药卫生—药学]