摘要
目的 :建立正常人血浆中克拉霉素浓度的LC MS测定方法。方法 :血浆样品经碱化后用乙醚提取 ,采用选择性离子检测方法测定其血药浓度。检测仪器为岛津LCMS 2 0 10四极杆质谱检测器 ,离子源为ESI源 ,检测离子 :克拉霉素m/z:748 5[M +H] + ,罗红霉素m/z :83 7 5[M +H ] + ,14 羟基克拉霉素m/z :764 5[M +H] + ;色谱柱为Shim packODS(5 0 μm ,2 50mm× 2 0mmI D ) ;流动相为 0 0 5%醋酸 乙腈 (40∶60v/v)。 结果 :克拉霉素的线性范围为 0 0 62 5～ 8 0 0 μg/ml ,方法的回收率为 86%～ 98% ,日内和日间的精密度均小于 17%。 结论 :该方法经考察符合血浆样品的测定要求 ,可以应用于临床血药浓度的测定和药代动力学研究。
AIM:To develop an LC-MS method for t he determination of clarithromycin concentration in human plasmaMETH OD:20 μl of roxithromycin solution(10 μg/ml,internal standard)was a dded to 020 ml of plasmaThe plasma samples were extracted with 4 ml ether a fter alkalizing using 01 mol/L Na 2CO 3Three ml of organic layer was transferred to clean tube and evaporated to dryness under N 2The res idue was reconstitued in 1 ml acetonitrile and 10 μl was injected into a n ODS C 18 (5 μm,250 mm×20 mm) columnThe mobile phase consisted of a cetonitrile:005% acetic acid (60∶40 v/v) at flow rate of 02 ml/min The eluate from the HPLC column was plumbed directly into ESI probe Analysis i n the mass spectrometer was operated in the selected-ion monitoring model The mass spectrometers was operated in SIM m/z 7485 for clarithromycin,837 5 for roxithromycin and 7645 for 14-hydroxylclarthromycin RESULT :Recoveries of clarithromycin at 0125,100 and 800 μg/ml were 865%,989% and 985% respectively The standard curve was linear in th e rang e of 00625～800 μg/ml The relative standard derivation of intra-day a nd in ter-day was smaller than 17% CONCLUSION: The me tho d of LC-MS is suitable for pharmacokinetic study of clarithromycin in human pla sma
出处
《中国药科大学学报》
CAS
CSCD
北大核心
2004年第1期50-53,共4页
Journal of China Pharmaceutical University
基金
国家 8 6 3计划 (编号 :2 0 0 3AA2Z34 7A)
江苏省药物代谢动力学重点实验室 (编号 :BM 2 0 0 1 2 0 1 )~~
