Rapid Simultaneous Determination of Amphetamine, Methamphetamine, 3,4-Methylenedioxyamphetamine, 3,4-Methylenedioxymethamphetamine, and 3,4-Methylenedioxyethylamphetamine in Urine by Fast Gas chromatography-mass Spectrometry

Abstract

The use of fast gas chromatography-mass spectrometry (FGC-MS) was investigated to improve the efficiency of analysis of urine specimens that previously screened presumptively positive for amphetamine (AMP), methamphetamine (MAMP), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), and/or 3,4 methylenedioxyethylamphetamine (MDEA) by immunoassay testing. Specimens were pretreated with basic sodium periodate, extracted using a positive-pressure manifold/cation-exchange solid-phase cartridge methodology, and derivatized using 4-carbethoxyhexafluorobutyryl chloride (4-CB). The analytical method was compared to traditional GC-MS analysis and evaluated with respect to assay chromatography, linearity, sensitivity, precision, accuracy, and reproducibility. The limits of detection were 62.5 ng/mL for MDA and 31.25 ng/mL for AMP, MAMP, MDMA, and MDEA. All of the target analytes were linear to 12,000 ng/mL with the exception of MAMP which was linear to 10,000 ng/mL. The intra-assay precision of a 500 ng/mL multiconstituent control (n=15) ranged from 522.6 to 575.9 ng/mL with a coefficient of variation of less than 3.8%. Authentic human urine specimens (n=187) previously determined to contain the target analytes were re-extracted and analyzed by both FGC-MS and the currently utilized GC-MS method. No significant differences in specimen concentration were observed between these analytical methods. No interferences were seen when the performance of the FGC-MS method was challenged with ephedrine, pseudoephedrine, phenylpropanolamine, and phentermine. When compared to traditional GC-MS analysis, FGC-MS analysis provided a dramatic reduction in retention time for amphetamine (1.8 min vs. 4.12 min). For example, the FGC-MS method reduced overall run time for a batch of 56 specimens from 12.0 h to 7.25 h. This reduction in analysis time makes FGC-MS an attractive alternative to traditional GC-MS by allowing a laboratory greater flexibility in the purchase and use of capital equipment and in the assignment of laboratory personnel, all resulting in greater overall efficiency by decreasing reporting times for AMP, MAMP, and designer amphetamine positive specimens.

Rapid GC–MS confirmation of amphetamines in urine by extractive acylation

“…A total instrumental cycle-time of 6 min per sample was obtained, which compares favourably with current rapid chromatographic methodologies for both GC-MS and LC-MS/MS [16,21]. The total sample preparation time for a batch of 20 specimens, performed by a single analyst, was approximately 45 min.…”

“…Analytical strategies including gas chromatography (GC) [12,13], high performance liquid chromatography (HPLC) [14,15], gas chromatography-mass spectrometry (GC-MS) [10,12,[16][17][18][19][20][21] and liquid chromatography-tandem mass spectrometry (LC-MS/MS) [22,23] have been employed. The majority of samples received by our laboratory are direct confirmation requests by clinicians.…”

“…Rapid chromatographic separation with microbore capillary columns [26] and quick temperature gradients [16,27] in fast GC-MS analysis have indicated the possibility of accurate quantitation in relatively short analysis times with adequate resolution between structurally close-related components. Care must, however, be taken in addressing the number of data points that define a chromatographic peak for forensic confirmations in such methodologies [28][29][30].…”

Direct Analysis of Conjugate Metabolites of Methamphetamine, 3,4-Methylenedioxymethamphetamine, and Their Designer Drugs in Biological Fluids

“…[18][19][20][21][22][23][24][25] Especially, the determinations of specific metabolites in addition to unchanged drugs provide absolute proof of drug intakes. MA, MDMA and their designer drugs are metabolized mainly to p-hydroxylated or demethylenated (followed by methylation) form as shown in Fig.…”

Determination of N-methyl-1-phenol-2-propanamine trace amounts in urine samples with molecular-imprinted polymer based sorbents

“…Так как N-метил-1-фе-нил-2-пропанамин представляет собой основание, то для его определения широкое распространение получили методы твердофазной экстракции (ТФЭ) с использованием катионобменных и смешанных сорбентов [4][5][6][7][8][9][10][11].…”