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[目的]建立一种简便、快速的液相-质谱联用(LC-MS/MS)法测定人血浆中的阿奇霉素浓度。[方法]采用API3000型LC-MS/MS液质联用系统,Ultimate C18分析柱(100×4.6mm,5μm),流动相为甲醇-水-甲酸(70︰30︰0.001,用氨水调pH=3.5),流速0.4ml·min-1。样品在碱性条件下用二氯甲烷提取浓集后进样,MRM模式检测(离子对794.5/591.4),莫沙比利(422.1/198.0)为内标,按内标法定量。[结果]阿奇霉素和内标的保留时间分别为2.8、3.6min,标准曲线在1～1024ng·ml-1范围内线性良好,最低定量限1ng·ml-1,日内、日间RSD分别小于6.6%和9.1%,方法回收率96.4%～108.9%,预处理回收率66.3～78.2%。[结论]本法具有快速简便、灵敏准确等特点,与已有文献报道相比有更好的灵敏度和特异性,适用于血浆中阿奇霉素含量测定及药代动力学、生物利用度研究用。
[Objective] To establish a simple and rapid liquid chromatography-mass spectrometry (LC-MS / MS) method for the determination of azithromycin in human plasma. [Method] The API3000 LC-MS / MS LC / MS system was used with the Ultimate C18 column (100 × 4.6 mm, 5 μm). The mobile phase consisted of methanol- water- 3.5), flow rate 0.4ml · min-1. Samples were extracted with dichloromethane and concentrated under basic conditions. The samples were detected by MRM (ion pair 794.5 / 591.4) and mosapride (422.1 / 198.0) as internal standard and quantified by internal standard method. [Results] The retention times of azithromycin and internal standard were 2.8 and 3.6 min, respectively. The calibration curve was linear over the range of 1 ~ 1024 ng · ml-1 with the lowest limit of quantitation of 1 ng · ml-1. The intra- and inter-day RSD were less than 6.6% 9.1%, the recovery rate of 96.4% ~ 108.9%, pretreatment recovery rate of 66.3 ~ 78.2%. [Conclusion] The method is rapid, simple, sensitive and accurate. It has better sensitivity and specificity than those reported in the literature and is suitable for the determination of azithromycin in plasma and pharmacokinetics and bioavailability.