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目的建立快速、灵敏的反相C_(18)色谱-质谱联用法测定沙丁胺醇气雾剂给药后在人体血浆中的浓度。方法血浆样品中加入沙丁胺醇-d9同位素内标,并经乙腈进行蛋白沉淀后,用Welch Ultimate XB-C_(18)色谱柱(2.1 mm×50 mm,5μm)经梯度洗脱被分离,流动相为乙腈(B)-5 mmol·L~(-1)乙酸铵的水溶液(含0.05%甲酸,A),流速为0.6 m L·min~(-1),进样量20μL,分析时间3 min。用电喷雾电离(ESI)源正离子模式、多反应监测(MRM),用于定量分析离子对分别是m/z240.1→m/z 148.1(沙丁胺醇)和m/z 249.1→m/z 149.1(沙丁胺醇-d9)。结果沙丁胺醇的线性范围为5~1500 pg·m L~(-1),定量下限为5 pg·m L~(-1),日内及日间精密度为2.70%~8.60%,回收率为99.02%~100.74%。结论本方法快速、灵敏且高效,适用于准确地测定人体血浆中沙丁胺醇的浓度。
OBJECTIVE To establish a rapid and sensitive reverse phase C_ (18) chromatography-mass spectrometry for the determination of the concentration of salbutamol aerosol in human plasma after administration. Methods Salbutamol-d9 internal standard was added to the plasma samples and precipitated by acetonitrile. The protein was separated by gradient elution on a Welch Ultimate XB-C 18 column (2.1 mm × 50 mm, 5 μm). The mobile phase was Acetonitrile (B) 5 mmol·L -1 ammonium acetate in water (containing 0.05% formic acid, A) at a flow rate of 0.6 m L · min -1 with a sample volume of 20 μL and an analysis time of 3 min. Electron spray ionization (ESI) source positive ion mode, multiple reaction monitoring (MRM) for quantitative analysis of ion pairs were m / z 240.1 → m / z 148.1 (albuterol) and m / z 249.1 → m / z 149.1 (Salbutamol-d9). Results The linear range of salbutamol was 5-1500 pg · m L -1 with the lower limit of quantitation of 5 pg · m L -1. The intra- and inter-day precision was 2.70% -8.60% and the recovery was 99.02 % ~ 100.74%. Conclusion The method is rapid, sensitive and efficient and suitable for the accurate determination of salbutamol in human plasma.