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目的建立LC-MS/MS法测定人血清中替加环素的浓度。方法人血清样品用乙腈沉淀蛋白后,选用Agilent Poreshell C_(18)(50 mm×3.0 mm,2.7μm)色谱柱,以乙腈-水(含0.03%三氟乙酸)为流动相梯度洗脱,流速为0.40 m L·min~(-1)。采用电喷雾离子化源,正离子方式,多反应监测(MRM)扫描方式进行监测。用于定量分析的离子反应分别为m/z 586.1→513.1(替加环素)和m/z 444.8→428.2(内标多西环素)。结果血清中替加环素的线性范围为0.02~2.5 mg·L~(-1)(r=0.997 9),定量下限为0.02 mg·L~(-1);低、中、高3种浓度下,本方法平均回收率为95.5%~104.1%,日内、日间精密度良好(RSD均<15%),提取回收率为86.8%~93.2%。结论该方法快速、灵敏、准确,专属性强,重复性好,适用于人血清中替加环素浓度的测定。
Objective To establish a method for the determination of tigecycline in human serum by LC-MS / MS. Methods Human serum samples were precipitated with acetonitrile, and then were separated on a Agilent Poreshell C_ (18) (50 mm × 3.0 mm, 2.7 μm) column using acetonitrile-water with 0.03% trifluoroacetic acid as mobile phase. The flow rate 0.40 m L · min -1. The electrospray ionization source, positive ion mode and multi-reaction monitoring (MRM) were used for monitoring. The ion reactions used for quantitative analysis were m / z 586.1 → 513.1 (tigecycline) and m / z 444.8 → 428.2 (internal standard doxycycline), respectively. Results The linear range of tigecycline in serum was 0.02-2.5 mg · L -1 (r = 0.997 9), and the lower limit of quantitation was 0.02 mg · L -1. The concentrations of tigecycline, , The average recovery of this method was 95.5% -104.1%, with good precision in both days and days (RSD <15%). The recovery rates ranged from 86.8% to 93.2%. Conclusion The method is rapid, sensitive, accurate, specific and reproducible. It is suitable for the determination of tigecycline in human serum.