Monolithic silica capillary column extraction of methamphetamine and amphetamine in urine coupled with thin-layer chromatographic detection (original) (raw)

Determination of Amphetamine and Methamphetamine by Dispersive Liquid Phase Micro-extraction: A Novel Experimental Approach

Iranian Journal of Toxicology, 2020

Background: A syringe to syringe dispersive liquid phase micro-extraction-floating organic drop was applied and used for the simultaneous extraction and pre-concentration of trace amounts of amphetamine (AMP) and methamphetamine (MAMP) in urine samples. The extracted analytes were determined by high performance liquid chromatography along with diode array detection. Methods: In this study, n-hexane was selected as the extraction solvent without the need to use dispersive solvent. The analytical parameters affecting the micro-extraction efficiency, including pH of sample solution, extraction solvent volume, the cycles of extraction and time of centrifugation were investigated and optimized by screening and optimization experimental design methods. Results: Underoptimal conditions, the calibration curve had a linear range of 2-100 μg/L with the determination coefficient of R2=99.8 and R2=99.6 for AMP and MAMP, respectively. The limit of detection was 2 μg/L for AMP and MAMP, and the ...

Development and Validation GC/MS Method for Methamphetamine Analysis in Urine by Miniaturization QuEChERS

Science and Technology Indonesia

This paper explains the development of a quick and easy gas chromatography (GC) approach to identify methamphetamine in urine. This research used gas chromatography with mass spectroscopy and a capillary column TG-5SILMS (5% phenyl methyl siloxane, 30 m x 0.32 x 25 m). The carrier gas flow rate was set at 1.0 mL/minute, the temperature inlet and detector had been set at 300°C, and the oven temperature was programmed to initiate at 50°C and held for 1.5 minutes before being raised to 300°C at a rate 40°C/minute and held for 3 minutes. Sample pre-treatment by modification of the QuEChERS method includes using a relatively large amount of inorganic salt, extraction volume and extraction cycle. The optimal conditions for processing a 400 uL urine sample were 160 mg magnesium sulphate, 40 mg sodium chloride, and 400 uL acetonitrile for organic solvent. According to the validation test, the detection limit for methamphetamine was 0.36 ug/mL; the quantitation limit was 1.09 ug/mL, and the ...