Simultaneous determination of amphetamine and related compounds in human urine using ultrasound-assisted emulsification microextraction and gas chromatography

Abstract

3,4-methylenedioxymethylamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxyethylamphetamine (MDEA) and 3,4-methylenedioxypropylamphetamine (MDPA) were extracted from human urine by using ultrasound-assisted emulsification microextraction (USAEME) method based on applying low density organic solvents followed by gas chromatographic analysis with flame ionization detection. Fourteen microliters of toluene was injected slowly into a 12 mL home-designed centrifuge glass vial containing a sample without salt addition that was located inside the ultrasonic water bath. The formed emulsion was centrifuged and 2 mL of separated toluene was injected into a gas chromatographic system equipped with a flame ionization detector (GC-FID) for analysis. In order to improve the extraction efficiency, experimental parameters affecting the extraction efficiency, including type and volume of extraction solvent, pH value of sample, extraction time and temperature were investigated. Under the optimal conditions, the linear dynamic range was in the range of 0.5-500 mg L À1 for MDEA and MDPA and 1.0-500 mg L À1 for MDA and MDMA with limits of detection (LODs) in the range of 0.2 to 0.4 mg L À1 . The results indicate that the developed method is rapid, accurate and sensitive and can be used for the simultaneous determination of MDA, MDMA, MDEA and MDPA in urine samples.

Application of Microextraction-Based Techniques for Screening-Controlled Drugs in Forensic Context—A Review

“…Table 3 summarizes in detail these miniaturized applications for the enrichment of amphetamine and related substances in forensic matrices, with emphasis on the key characteristics on the developed methodologies. Table S3 (Supplementary Material) contains information regarding other techniques for the determination of these classes of compounds in the forensic context [ 40 , 89 , 90 , 91 , 92 , 93 , 94 , 95 , 96 , 97 , 98 , 100 , 104 , 105 , 129 , 130 , 131 , 140 , 141 , 142 , 143 , 144 , 145 , 146 , 147 , 148 , 149 , 150 , 151 , 152 , 153 , 154 , 155 , 156 , 157 , 158 , 159 , 160 , 161 , 162 , 163 , 164 , 165 , 166 , 167 , 168 , 169 ...…”

Review on analytical methods for quantification of ADHD drugs in human biological samples

“…The column, injector and detector temperature were set at 140°C to 270°C, 250°C, 300°C, respectively and detection was using NPD [179]. Other GC methods for the quantification of AMP and MPH in human biological samples [180][181][182][183][184][185][186][187][188] are reported in Table 3.…”

Fast Dispersive Liquid-Liquid Microextraction Based on Temperature Switching Deep Eutectic Solvent as A Green Extractant

“…Dispersive liquid-liquid microextraction (DLLME) is an e cient and fast liquid-phase microextraction method proposed by Rezaee (Rezaee, et al, 2006) in 2006. The main improvement work is concentrated on innovating the dispersion method (Psillakis, 2019;Saleh, et al, 2009;Zhong, et al, 2019), updating the phase separation method (Guo, et al, 2016;Ngaosi, et al, 2016;Rezaee, et al, 2012;Ye, et al, 2016;Zhong, et al, 2019), and the usage of low-toxic extractants as much as possible. The ionic liquid (Marcinkowska, et al, 2019) which was used to replace the toxic extractant in DLLME (Montalbán, et al, 2018;Wu, et al, 2013) was found to be harmful to environment recently (Montalbán, et al, 2018).…”