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采用填充吸附剂微萃取结合液相色谱 - 电喷雾电离串联质谱法测定犬血浆样品中的AZD6118。

Determination of AZD6118 in dog plasma samples utilizing microextraction by packed sorbent and liquid chromatography-electrospray ionization tandem mass spectrometry.

作者信息

El Beqqali Aziza, Ahmadi Mazaher, Abdel-Rehim Mohamed

机构信息

Department of Environmental Sci. & Analytical Chemistry, Stockholm University, SE10691 Stockholm, Sweden.

Department of Environmental Sci. & Analytical Chemistry, Stockholm University, SE10691 Stockholm, Sweden.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Feb 1;1043:20-24. doi: 10.1016/j.jchromb.2016.11.004. Epub 2016 Nov 4.

Abstract

In this work, for the first time, a method has been developed for the determination of AZD6118, a candidate drug, in dog plasma samples. The method is based on microextraction by packed sorbent (MEPS) of the drug prior to liquid chromatography-electrospray ionization tandem mass spectrometry assay. Various important factors affecting MEPS performance were optimized, and under the optimized condition, a linear calibration curve in the concentration range of 20-25,000nmolL with a coefficient of determination over 0.99 was obtained. The back-calculated values of the calibration points showed good agreement with the theoretical concentrations (coefficients of variation percent between 0.3-3.8). The lower limit of quantification and limit of detection were 20.0 and 2.9nmolL, respectively. The repeatability and accuracy of the method was evaluated by determination of quality control samples at three concentration levels (low, medium and high) using the developed method, and the results (coefficients of variation values were between 1.9% and 3.2%, relative recoveries ranged between 93.5-102.1%) confirm that a powerful method has been developed for the extraction and determination of the investigated drug in dog plasma.

摘要

在本研究中,首次开发了一种用于测定犬血浆样本中候选药物AZD6118的方法。该方法基于在液相色谱-电喷雾电离串联质谱分析之前,通过填充吸附剂微萃取(MEPS)对药物进行萃取。对影响MEPS性能的各种重要因素进行了优化,在优化条件下,获得了浓度范围为20-25,000nmol/L、决定系数超过0.99的线性校准曲线。校准点的反算值与理论浓度显示出良好的一致性(变异系数百分比在0.3-3.8之间)。定量下限和检测限分别为20.0和2.9nmol/L。使用所开发的方法,通过测定三个浓度水平(低、中、高)的质量控制样品来评估该方法的重复性和准确性,结果(变异系数值在1.9%至3.2%之间,相对回收率在93.5-102.1%之间)证实已开发出一种用于在犬血浆中萃取和测定所研究药物的有效方法。

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