• 主题
高级搜索  >
历史搜索 清空历史
首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >A novel and sensitive method for ethinylestradiol quantification in human plasma by high-performance liquid chromatography coupled to atmospheric pressure photoionization (APPI) tandem mass spectrometry: Application to a comparative pharmacokinetics study
【24h】

A novel and sensitive method for ethinylestradiol quantification in human plasma by high-performance liquid chromatography coupled to atmospheric pressure photoionization (APPI) tandem mass spectrometry: Application to a comparative pharmacokinetics study

机译：高效液相色谱-大气压光电离（APPI）串联质谱联用测定人血浆中乙炔雌二醇的新颖灵敏方法：在比较药代动力学研究中的应用

获取原文
获取原文并翻译 | 示例
           
页面导航
  • 摘要
  • 著录项
  • 相似文献
  • 相关主题

摘要

In the present Study, a novel, fast, sensitive and robust method to quantify ethinylestradiol in human plasma using 17 alpha-ethinylestradiol-d4 as the internal standard (IS) is described. The analyte and the IS were extracted from acidified plasma by liquid-liquid extraction (LLE) using diethyl ether-hexane followed by online solid phase extraction (SPE) using online C18 cartridges. Extracted samples were analyzed by high-performance liquid chromatography coupled to atmospheric pressure photoionization tandem mass spectrometry (HPLC-APPI-MS/MS). Chromatography was performed isocratically on a C18, 5 mu m analytical column. The method had a chromatographic run time of 2.50 min and a linear calibration Curve over the range 5-500 pg ml(-1) (r(2) > 0.9992). The lowest concentration quantified was 5 pg ml(-1), demonstrating acceptable accuracy and precision. The intra-assay precisions ranged from 2.1 to 14.6%. while inter-assay precisions ranged from 4.4 to 11.4%. The intra-assay accuracies ranged from 94.6 to 103.8%, while the inter-assay accuracies ranged from 98.9 to 101.6%. The recovery of ethinylestradiol was determined as part of the assay validation process and was 73.1 and 79.0% for the concentrations 15 and 375 pg ml(-1). respectively. Short-term stability showed that ethinylestradiol was stable in plasma for at least 19 h at room temperature or for at least 385 days when stored at -20 degrees C. In the study of bioequivalence conducted in Brazil, healthy Volunteers received two ethinylestradiol 0.035 mg tablet formulations using an open, randomized, two-period crossover design with a 2-week washout interval. Since the 90% confidence interval for C-max and area under the curve ratios were all inside the 80-125% interval proposed by the US Food and Drug Administration, it was concluded that the two ethinylestradiol formulations are bioequivalent with respect to both the rate and the extent of absorption.
机译：在本研究中，描述了一种新颖，快速，灵敏且稳定的方法，使用17α-乙炔雌二醇-d4作为内标（IS）定量测定人血浆中乙炔雌二醇。使用二乙醚-己烷通过液-液萃取（LLE）从酸化血浆中萃取分析物和IS，然后使用在线C18色谱柱在线固相萃取（SPE）。萃取的样品通过高效液相色谱与大气压光电离串联质谱联用（HPLC-APPI-MS / MS）进行分析。色谱法在5毫米C18分析柱上等度地进行。该方法的色谱运行时间为2.50分钟，线性校准曲线在5-500 pg ml（-1）范围内（r（2）> 0.9992）。定量的最低浓度为5 pg ml（-1），表明可接受的准确性和精密度。批内精密度范围从2.1到14.6％。批间准确度在4.4％至11.4％之间。批内准确性从94.6％到103.8％，批间准确性从98.9％到101.6％。乙炔雌二醇的回收率是测定验证过程的一部分，对于15和375 pg ml（-1）的浓度，回收率为73.1％和79.0％。分别。短期稳定性显示，乙炔雌二醇在室温下至少在血浆中稳定19小时，或在-20摄氏度下保存至少385天。在巴西进行的生物等效性研究中，健康志愿者接受了两次乙炔雌二醇0.035毫克片剂使用开放的，随机的，两阶段交叉设计的制剂，洗脱间隔为2周。由于C-max的90％置信区间和曲线比率下的面积均在美国食品药品监督管理局提议的80-125％区间内，因此得出结论，两种炔雌醇制剂在两种比率上均具有生物等效性。和吸收程度。

著录项

相似文献

  • 外文文献
  • 中文文献
  • 专利
获取原文

客服邮箱：kefu@zhangqiaokeyan.com

京公网安备：11010802029741号 ICP备案号：京ICP备15016152号-6 六维联合信息科技 (北京) 有限公司©版权所有

  • 客服微信

  • 服务号