液相色谱-离子阱质谱法测定人血清中莫西沙星浓度

目的建立一种灵敏、可靠的检测血清中莫西沙星浓度的高效液相色谱-离子阱质谱法。方法血清样品经磷酸盐缓冲液提取后，用Waters Oasis MAX小柱进行净化，以乙腈-0．05％三氟醋酸（25：75，V／V）为流动相，采用Cloversil—C18柱（150mm×3．0mm，5μm）分离，以环丙沙星为内标，应用高效液相色谱-电喷雾离子阱质谱多离子反应监测模式（MRM）测定，莫西沙星和内标的定量离子对分别为m／z402→358和m／z332→288。结果莫西沙星和内标的绝对回收率均为83．1％→90．7％，莫西沙星质量浓度为0．5-100．0μg·L^-1具有良好线性，日内精密度〈7．2％，日间精密度〈9．8％，检出限为0．5μg·L^-1。结论本方法简便、灵敏、干扰少、特异性好，可用于莫西沙星的临床药动学研究及临床患者的血药浓度测定。

Determination of concentration of moxifloxacin in human serum by high-performance liquid chromatography coupled with ion trap mass spectrometry

AIM To develop a sensitive and accurate method for the determination of moxifloxacin in human serum by high-performance liquid chromatography coupled with ion trap mass spectrometry （HPLC-ITMS）. METHODS Mter moxifloxacin in human serum was extracted by phosphate buffer, the sample was cleaned with solid-phase extraction （SPE） using Oasis MAX cartridges. The separation was performed on a Cloversil-C18 column（ 150 mm × 3.0 mm, 5 μm）using the mobile phase consisting of acetonitrile- 0.05% trifluoroacetic acid （25/75, V/ V）. Detection was carried out by a positive electrospray ionization in the multiple reaction monitoring （MRM） mode with the transitions of m/z 402→358 and m/z 332→288 for moxifloxacin and ciprofloxacin （an internal standard）, respectively. RESULTS Calibration curve was linear within the range of 0.5 - 100.0μg·L^-1, and the extraction recoveries were from 80.5% to 86.0%. The intra-day RSD was less than 7.2%, and the inter-day RSD was less than 9.8%. The detection limit was 0.5 μg· L^-1 for moxifloxacin. CONCLUSION This method is found to be simple, sensitive, little interferential and good specificity for pharmacokinetic studies and the determination of moxifloxacin in human serum for patients.