Gas chromatography‐mass spectrometric method for the screening and quantification of illicit drugs and their metabolites in human urine using solid‐phase extraction and trimethylsilyl derivatization

Abstract

A simple and rapid GC-MS method has been developed for the screening and quantification of many illicit drugs and their metabolites in human urine by using automatic SPE and trimethylsilylation. Sixty illicit drugs, including parent drugs and their metabolites that are possibly abused in Korea, can be monitored by this method. Among them, 24 popularly abused illicit drugs were selected for quantification. Very delicate optimizations were carried out in SPE, trimethylsilylation derivatization, and GC/MS to enable such remarkable achievements. Trimethylsilylated analytes were well separated within 21 min by GC-MS. In the validation results, the LOD of all the analytes were in the range of 2-75 ng/mL. The LOQ of the quantified analytes were in the range of 5-98 ng/mL. The linearity (r(2)) of the quantified analytes ranged 0.990-1.000 in each concentration range between 10 and 1000 ng/mL. The mean recoveries ranged from 62 to 126% at three different concentrations of each analyte. The inter-day and inter-person accuracies were within -13.3 approximately 14.9%, and -10.1 approximately 13.0%, respectively, and the inter-day and inter-person precisions were less than 12.9%. The method was reliable and efficient for the screening and quantification of abused illicit drugs in routine urine analysis.

Conjugation of nitrated acetaminophen to Der p1 amplifies peripheral blood monocyte response to Der p1

“…Samples were analyzed in Scan mode using electron impact ionization (EI). Ion dwell time was set to 10 msec [ 33 ]. Samples were analyzed with electron impact ionization.…”

Clinical Application Study of Polymeric Nanospheres Network in Methylphenidate Extraction from Urine Samples by Dispersive Solid Phase Extraction Adsorbent

“…MPH was extracted and screened by derivatization and SPE steps coupled with gas chromatography mass spectrometry (GC-MS) in urine media (4). Automatic SPE and trimethylsilylation sample preparation method coupled with GC-MS was introduced for extraction and determination of MPH from humane urine (16). However, Enantioseparation of MPH was carried out using a chiral fluorescent derivatization reagent in rat plasma (17).…”

Analysis of a new drug of abuse: Cathinone derivative 1‐(3,4‐dimethoxyphenyl)‐2‐(ethylamino)pentan‐1‐one

“…Distribution of the pure effective enantiomer by providers can lead to overdose or in the worst cases even to the death of the consumer. Due to these facts not only identification and separation of the pure compound is necessary, but also blood and urine analysis . The naturally occurring ( S )‐cathinone appeared on the European and American drug market recently masked as e.g.…”