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目的建立高效液相色谱-质谱联用法测定血浆中奥替溴铵浓度的方法。方法采用Eclipse Plus C18(150mm×2.1mm,3.5μm)色谱柱,柱温30℃,流动相为乙腈-20mmol/L-醋酸铵-乙酸溶液(58:42:0.1,V/V),流速0.35ml/min,电喷雾离子源,正离子检测,检测对象为奥替溴铵和内标氯苄律定的m/z分别为483.3和464.1。结果奥替溴铵和氯苄律定的保留时间分别为5.1min和2.0min,奥替溴铵在0.1-20.0μg/L浓度范围内有良好的线性关系(r=0.9998),定量下限为0.1μg/L,批内和批间精密度的相对标准偏差均小于15%,相对回收率93%-97%%。结论高效液相色谱-质谱联用测定准确、灵敏、简便,可用于人血浆的奥替溴铵浓度检测。
Objective To establish a method for the determination of otibromide in plasma by high performance liquid chromatography-mass spectrometry. Methods The chromatographic column was Eclipse Plus C18 (150 mm × 2.1 mm, 3.5 μm). The mobile phase consisted of acetonitrile-20 mmol / L ammonium acetate-acetic acid solution (58:42: 0.1, V / V) ml / min, electrospray ionization, positive ion detection, the test object for the oltibium bromide and internal standard law of benzyl clonazepam m / z 483.3 and 464.1 respectively. Results The retention times of oltipraz and benzyl chloride were 5.1 min and 2.0 min, respectively. There was a good linearity (r = 0.9998) of the etiotridium bromide in the concentration range of 0.1-20.0 μg / L, and the lower limit of quantitation was 0.1 μg / L. The relative standard deviations (RSDs) within and between batches were less than 15% and the relative recoveries were 93% -97 %%. Conclusion High performance liquid chromatography-mass spectrometry (HPLC-MS) is accurate, sensitive and simple and can be used to detect the concentration of Otibromide in human plasma.