Combined administration of fluticasone propionate and salmeterol xinofoate has been widely used for the treatment of asthma in recent decades. In this investigation, we developed and validated a novel and sensitive ul...Combined administration of fluticasone propionate and salmeterol xinofoate has been widely used for the treatment of asthma in recent decades. In this investigation, we developed and validated a novel and sensitive ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method for simultaneous determination of fluticasone propionate and salmeterol xinofoate in human plasma. Following a simple SPE sample extraction in 96-well plate format, chromatography was performed on a Waters ACQUITY UPLC BEH C 18 column （1.7 μm, 50 min×2.1 mm） with mobile phase consisting of 100% MeOH and 0.1% NH4OH in water on a gradient program at flow rate of 0.5 mL/min. Detection of analytes and internal standards was accomplished using multiple reaction monitoring （MRM） of precursor〉product ion pairs of m/z 501.4〉313.2 （fluticasone propionate）, 506.4〉293.3 （fluticasone propionate-d5）, 416.4〉232.1 （salmeterol xinofoate） and 419.3〉235.2 （salmeterol-d3）. The assay range was 2.50-500 pg/mL for both analytes, and a 1/x2 weighted linear regression model was used. The inter-assay accuracy and precision of the method were within ±8.6%. The recoveries from 0.30 mL of plasma were greater than 51.0% and 54.6% for fluticasone propionate and salmeterol, respectively, and the results were consistent across low, middle and high concentration levels. The method was validated following FDA, EMA and CFDA （China Food and Drug Administration）＇s guidance on bioanalysis and then successfully applied to support a clinical study in healthy Chinese subjects following inhaled administration of a single combination of fluticasone propionate/salmeterol （250 μg/50 μg）.展开更多
目的：建立HPLC-MS/MS法测定人血浆中曲唑酮的浓度。方法：血浆样品经蛋白质沉淀法进行前处理后,以甲醇-水-醋酸铵-甲酸为流动相体系梯度洗脱,采用CAPCELL PAK C18MG色谱柱分离,流速为0.4ml/min,柱温为50℃。采用正离子多反应监测模式...目的：建立HPLC-MS/MS法测定人血浆中曲唑酮的浓度。方法：血浆样品经蛋白质沉淀法进行前处理后,以甲醇-水-醋酸铵-甲酸为流动相体系梯度洗脱,采用CAPCELL PAK C18MG色谱柱分离,流速为0.4ml/min,柱温为50℃。采用正离子多反应监测模式进行监测,以电喷雾离子源作为电离技术。结果：曲唑酮浓度在10.0~3000ng/ml范围内线性关系良好（r=0.996 9）,平均提取回收率为97.5%,批内、批间RSD均≤8.2%（n=6）。结论：此方法专属、灵敏、准确、简单、快速,适用于曲唑酮临床生物样本的分析和研究。展开更多
文摘Combined administration of fluticasone propionate and salmeterol xinofoate has been widely used for the treatment of asthma in recent decades. In this investigation, we developed and validated a novel and sensitive ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method for simultaneous determination of fluticasone propionate and salmeterol xinofoate in human plasma. Following a simple SPE sample extraction in 96-well plate format, chromatography was performed on a Waters ACQUITY UPLC BEH C 18 column （1.7 μm, 50 min×2.1 mm） with mobile phase consisting of 100% MeOH and 0.1% NH4OH in water on a gradient program at flow rate of 0.5 mL/min. Detection of analytes and internal standards was accomplished using multiple reaction monitoring （MRM） of precursor〉product ion pairs of m/z 501.4〉313.2 （fluticasone propionate）, 506.4〉293.3 （fluticasone propionate-d5）, 416.4〉232.1 （salmeterol xinofoate） and 419.3〉235.2 （salmeterol-d3）. The assay range was 2.50-500 pg/mL for both analytes, and a 1/x2 weighted linear regression model was used. The inter-assay accuracy and precision of the method were within ±8.6%. The recoveries from 0.30 mL of plasma were greater than 51.0% and 54.6% for fluticasone propionate and salmeterol, respectively, and the results were consistent across low, middle and high concentration levels. The method was validated following FDA, EMA and CFDA （China Food and Drug Administration）＇s guidance on bioanalysis and then successfully applied to support a clinical study in healthy Chinese subjects following inhaled administration of a single combination of fluticasone propionate/salmeterol （250 μg/50 μg）.
文摘目的：建立HPLC-MS/MS法测定人血浆中曲唑酮的浓度。方法：血浆样品经蛋白质沉淀法进行前处理后,以甲醇-水-醋酸铵-甲酸为流动相体系梯度洗脱,采用CAPCELL PAK C18MG色谱柱分离,流速为0.4ml/min,柱温为50℃。采用正离子多反应监测模式进行监测,以电喷雾离子源作为电离技术。结果：曲唑酮浓度在10.0~3000ng/ml范围内线性关系良好（r=0.996 9）,平均提取回收率为97.5%,批内、批间RSD均≤8.2%（n=6）。结论：此方法专属、灵敏、准确、简单、快速,适用于曲唑酮临床生物样本的分析和研究。
