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目的:建立高效液相色谱-质谱联用法测定人血浆中氨溴索浓度的方法。方法:血浆样品经NaOH碱化,乙醚提取浓缩后,以乙腈-水(85:15)为流动相,流速:0.2 mL·min~(-1),采用电喷雾离子源(ESI),以多离子反应监测方式(MRM)进行正离子检测,氨溴索和内标地西泮的定量分析离子对分别为m/z 378.9→263.9和m/z 285.1→193.1。结果:血浆样品中氨溴索线性范围0.26～200μg·L~(-1)(r=0.9998),最低定量限为0.26ng·mL~(-1)。低、中、高(0.78,12.5,100μg·L~(-1))3种浓度的日内RSD分别为9.1%,8.3%和2.7%;日间RSD分别为10.0%,7.2%和12.4%;准确度为109%,114%和106%。结论:本方法灵敏度高、专属性强、重现性好、准确,可用于人血浆中氨溴索的含量测定。
Objective: To establish a method for the determination of ambroxol in human plasma by high performance liquid chromatography-mass spectrometry. Methods: The plasma samples were alkalized by NaOH and extracted with ether. The mobile phase consisted of acetonitrile - water (85:15), flow rate 0.2 mL · min ~ (-1), electrospray ionization (ESI) Ion pair reaction monitoring (MRM) was used for positive ion detection. The quantitative ionization pairs of ambroxol and internal standard diazepam were m / z 378.9 → 263.9 and m / z 285.1 → 193.1, respectively. Results: The linear range of ambroxol was 0.26 ~ 200 μg · L -1 (r = 0.9998) in plasma and the lowest limit of quantification was 0.26 ng · mL -1. The intra-day RSD of low, medium and high concentrations (0.78,12.5,100μg · L -1) were 9.1%, 8.3% and 2.7% respectively; the daytime RSD were 10.0%, 7.2% and 12.4% respectively; The accuracy is 109%, 114% and 106%. Conclusion: The method has high sensitivity, specificity, reproducibility and accuracy and can be used for the determination of ambroxol in human plasma.