Katselou Maria, Athanaselis Sotiris, Nikolaou Panagiota, Dona Artemisia, Spiliopoulou Chara, Papoutsis Ioannis
Department of Forensic Medicine and Toxicology, Faculty of Medicine, National and Kapodistrian University of Athens, Greece.
Department of Forensic Medicine and Toxicology, Faculty of Medicine, National and Kapodistrian University of Athens, Greece.
J Pharm Biomed Anal. 2017 Oct 25;145:765-772. doi: 10.1016/j.jpba.2017.07.059. Epub 2017 Aug 1.
A simple, rapid, sensitive and accurate gas chromatography-mass spectrometric method was developed and validated for the simultaneous determination of hydroxyzine and cetirizine in whole blood. Solid-phase extraction procedure using Bond Elut LRC Certify II columns was used for the isolation of hydroxyzine and cetirizine from 1mL whole blood followed by derivatization with a mixture of acetic anhydride:n-propanol (1:1, v/v). Limits of detection and quantification were 1.50 and 5.00ng/mL, respectively. The assay was linear within the concentration range of 5.00-1000.0ng/mL and the correlation coefficient was R≥0.993 for both analytes. Absolute recovery was determined at three quality control concentration levels and was found to be at least 87.2% for both substances. Intra-day and inter-day accuracy values for both hydroxyzine and cetirizine were ranged from -1.2 to 3.8% and -2.7 to 2.0%, respectively, at the three concentration levels studied, whereas their respective intra-day and inter-day precision values were less than 9.9 and 6.5%, respectively, in terms of relative standard deviation (%RSD). The developed method was successfully applied for the quantification of hydroxyzine and cetirizine concentrations in whole blood, during the investigation of clinical cases where these two antihistamines were detected.
建立并验证了一种简单、快速、灵敏且准确的气相色谱 - 质谱法，用于同时测定全血中的羟嗪和西替利嗪。采用Bond Elut LRC Certify II柱的固相萃取程序从1mL全血中分离羟嗪和西替利嗪，随后用乙酸酐 - 正丙醇（1:1，v/v）混合物进行衍生化。检测限和定量限分别为1.50和5.00ng/mL。该测定法在5.00 - 1000.0ng/mL的浓度范围内呈线性，两种分析物的相关系数均为R≥0.993。在三个质量控制浓度水平下测定了绝对回收率，两种物质的绝对回收率均至少为87.2%。在所研究的三个浓度水平下，羟嗪和西替利嗪的日内和日间准确度值分别为 - 1.2%至3.8%和 - 2.7%至2.0%，而它们各自的日内和日间精密度值，以相对标准偏差（%RSD）计，分别小于9.9%和6.5%。在检测到这两种抗组胺药的临床病例调查中，所建立的方法成功应用于全血中羟嗪和西替利嗪浓度的定量分析。
