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采用气相色谱 - 火焰离子化检测法快速测定血清和尿液中的乙二醇、1,2 - 丙二醇及乙醇酸用于急诊和临床毒理学检测

Fast determination of ethylene glycol, 1,2-propylene glycol and glycolic acid in blood serum and urine for emergency and clinical toxicology by GC-FID.

作者信息

Hložek Tomáš, Bursová Miroslava, Čabalaa 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

Talanta. 2014 Dec;130:470-4. doi: 10.1016/j.talanta.2014.07.020. Epub 2014 Jul 15.

Abstract

A simple, cost effective, and fast gas chromatography method with flame ionization detection (GC-FID) for simultaneous measurement of ethylene glycol, 1,2-propylene glycol and glycolic acid was developed and validated for clinical toxicology purposes. This new method employs a relatively less used class of derivatization agents - alkyl chloroformates, allowing the efficient and rapid derivatization of carboxylic acids within seconds while glycols are simultaneously derivatized by phenylboronic acid. The entire sample preparation procedure is completed within 10 min. To avoid possible interference from naturally occurring endogenous acids and quantitation errors 3-(4-chlorophenyl) propionic acid was chosen as an internal standard. The significant parameters of the derivatization have been found using chemometric procedures and these parameters were optimized using the face-centered central composite design. The calibration dependence of the method was proved to be quadratic in the range of 50-5000 mg mL(-1), with adequate accuracy (92.4-108.7%) and precision (9.4%). The method was successfully applied to quantify the selected compounds in serum of patients from emergency units.

摘要

开发并验证了一种简单、经济高效且快速的带有火焰离子化检测的气相色谱法(GC-FID),用于同时测定乙二醇、1,2-丙二醇和乙醇酸,以用于临床毒理学目的。这种新方法采用了一类相对较少使用的衍生化试剂——氯甲酸烷基酯,能在数秒内实现羧酸的高效快速衍生化,同时二醇类物质由苯硼酸进行衍生化。整个样品制备过程在10分钟内完成。为避免天然存在的内源性酸可能产生的干扰和定量误差,选择3-(4-氯苯基)丙酸作为内标。使用化学计量学方法确定了衍生化的重要参数,并采用面心中心复合设计对这些参数进行了优化。该方法的校准依赖性在50 - 5000 mg mL(-1)范围内被证明为二次关系,具有足够的准确度(92.4 - 108.7%)和精密度(9.4%)。该方法已成功应用于定量急诊科患者血清中的选定化合物。

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