气相色谱-火焰离子化检测法同时快速测定人血清中布洛芬、酮洛芬和萘普生用于临床毒理学研究
Fast ibuprofen, ketoprofen and naproxen simultaneous determination in human serum for clinical toxicology by GC-FID.
作者信息
Hložek Tomáš, Bursová Miroslava, Cabala Radomír
机构信息
Institute of Forensic Medicine and Toxicology, First Faculty of Medicine, Charles University in Prague and General University Hospital, 121 08 Prague 2, Czech Republic.
Institute of Forensic Medicine and Toxicology, First Faculty of Medicine, Charles University in Prague and General University Hospital, 121 08 Prague 2, Czech Republic; Department of Analytical Chemistry, Faculty of Science, Charles University in Prague, Albertov 6, 128 43 Prague 2, Czech Republic.
出版信息
Clin Biochem. 2014 Oct;47(15):109-11. doi: 10.1016/j.clinbiochem.2014.06.076. Epub 2014 Jul 6.
OBJECTIVES
The aim of this study was to develop and validate a gas chromatographic method with flame ionization detection (GC-FID) for the measurement of ibuprofen, naproxen and ketoprofen for clinical toxicology purposes.
DESIGN AND METHODS
100μL of plasma was treated with methyl chloroformate and derivatized analytes were extracted with hexane. Optimal conditions of the derivatization procedure have been found using the experimental chemometric design (face-centered central composite design). The selectivity and efficiency of the procedure was confirmed by GC-MS.
RESULTS
The assay was linear in the concentration range of 10-400μgmL(-1), with adequate accuracy and precision for GC-FID (98-106.7%, CV≤9.1%, respectively) and for GC-MS (99.3-105.5%, CV≤9.2%, respectively).
CONCLUSION
The entire sample preparation procedure is completed within 5 min and the quantitative results are available within 35 min. The method was successfully applied to quantify the selected compounds in serum of patients from emergency units.
目的
本研究的目的是开发并验证一种采用火焰离子化检测的气相色谱法（GC-FID），用于临床毒理学目的下布洛芬、萘普生和酮洛芬的测定。
设计与方法
用氯甲酸甲酯处理100μL血浆，并用己烷萃取衍生化后的分析物。使用实验化学计量学设计（面心中央复合设计）找到了衍生化程序的最佳条件。该程序的选择性和效率通过GC-MS得到了证实。
结果
该测定在10-400μgmL(-1)浓度范围内呈线性，对于GC-FID具有足够的准确度和精密度（分别为98-106.7%，CV≤9.1%），对于GC-MS也具有足够的准确度和精密度（分别为99.3-105.5%，CV≤9.2%）。
结论
整个样品制备过程在5分钟内完成，定量结果在35分钟内可得。该方法成功应用于急诊室患者血清中所选化合物的定量分析。
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