乙胺丁醇吡嗪酰胺和左氧氟沙星的浓度.docVIP

LC－MS/MS方法同时检测人血浆中异烟肼、利福平、乙胺丁醇、吡嗪酰胺和左氧氟沙星的浓度 赵冠人，彭明丽，申　健，栾潇潇，西 娜（解放军309医院药剂科，北京 100091） 摘要 目的方法Agilent Poroshell 120SB C18色谱柱（4.6 mm×50 mm，2.7 μm）为分析柱，ZORBAX SB C18柱（2.1 mm×12.5 mm，5μm）为保护柱，以0.2%甲醇-0.2%醋酸溶液为流动相，梯度洗脱，使用离子喷雾离子化源（ESI），以正离子多反应监测（MRM）方式进行检测，异烟肼m/z 138.0→121.0，利福平m/z 823.2→791.2，乙胺丁醇m/z 205.2→116.1，吡嗪酰胺m/z 124.1→79.0，左氧氟沙星m/z 362.2→261.1，对乙酰氨基酚m/z 152.0→110.0。分析时间为12 min。结果：血浆中内源性物质对测定无干扰，异烟肼、利福平、乙胺丁醇、吡嗪酰胺、左氧氟沙星的线性范围分别为0.20 ~ 9.81 μg·mL-1、0.60 ~ 30.12 μg·mL-1、0.10 ~ 4.89 μg·mL-1、1.01 ~ 50.6 μg·mL-1、0.10 ~ 5.00 μg·mL-1。批内、批间精密度（RSD）均小于10%，准确度（RE）均小于10%。结论：本方法特异性强，灵敏度高，测定结果可靠，适用于临床血浆样品的高通量分析。 [关键词]　异烟肼；利福平；乙胺丁醇；吡嗪酰胺；左氧氟沙星；高效液相色谱串联质谱；血药浓度监测 LC-MS/MS determination of isoniazid, rifampicin, ethambutol, pyrazinamide and levofloxacin in human plasma ZHAO Guan-ren, PENG Ming-li, SHEN Jian, LUAN Xiao-xiao，XI Na(Department of Pharmacy, the 309th Hospital of PLA, Beijing 100091, China） Abstract Objective:To establish an LC-MS/MS method for the determination of isoniazid，rifampicin，ethambutol，pyrazinamide and levofloxacin in human plasma. Methods: ?4-acetamidophenol was used as internal standard．The protein of plasma samples were precipitated with methanol．The supernatant was separated on an Agilent Poroshell 120SB C18 column(4.6mm×50 mm， 2.7μm)guarded by a ZORBAX SB-Aq column(2.1 mm×12.5 mm，5μm)．The mobile phase consisted of 0.2% methanol and 0.2% acetic acidc，gradient elution.Electrospray ionization(ESI)source was applied and operated in the positive multiple reaction monitoring(MRM)mode．The transition of m/z was 138.0→121.0 for isoniazid，823.2→791.2 for rifampicin，205.2→116.1 for ethambutol，124.1→79.0 for pyrazinamide，362.2→261.1 for levofloxacin and 152.0→110.0 for 4-acetamidophenol．Each analysis was completed within 12 min．Results:Chromatograms showed no endogenous interfering peaks with blank samples．The linear calibration curve was obtained within the range of 0.20~9.81 μg·mL-1 for isoniazid，0.60~30.12 μg·mL-1 for rifampicin，0.10~4.89 μg·mL-1 for ethambutol