期刊
MICROCHEMICAL JOURNAL
卷 124, 期 -, 页码 188-194出版社
ELSEVIER
DOI: 10.1016/j.microc.2015.07.028
关键词
Methylmalonic acid; Ultrasound-assisted emulsification microextraction; Gas chromatography-flame ionization detection; Urine analysis
资金
- Department of Chemistry, Boroujerd Branch, Islamic Azad University
An efficient microextraction technique followed by gas chromatography-flame ionization detector (GCFID) analysis was developed for determination of methylmalonic acid (MMA) concentration in human urine samples. This method was based on ultrasound-assisted emulsification microextraction followed by derivatization with a low density alcoholic solvent which performs both as an extraction solvent and as a derivatization agent, simultaneously. In this procedure, 80 mu L. of 1-heptanol was injected slowly into a 10 mL acidified aqueous sample of MMA placed inside an ultrasonic water bath. The resulting emulsion was centrifuged and after derivatization, 2 mu L. of the organic phase was injected into a GC-FID. Several factors affecting the derivatization and the extraction were optimized. Under the optimal conditions, linearity was in the range of 1 to 250 and 3 to 200 mu mol/L corresponding to the limits of detection (LOD) 0.8 and 2.4 mu mol/L in water and urine samples, respectively. The inter-day and intra-day precision of the proposed method were evaluated in terms of the relative standard deviation (RSD), which were <11% (n = 4). The proposed method presented an acceptable LOD for urinary MMA analysis with satisfactory RSD. (C) 2015 Elsevier B.V. All rights reserved.
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