Screening for illicit and medicinal drugs in whole blood using fully automated SPE and ultra‐high‐performance liquid chromatography with TOF‐MS with data‐independent acquisition

Abstract

A broad forensic screening method for 256 analytes in whole blood based on a fully automated SPE robotic extraction and ultra-high-performance liquid chromatography (UHPLC) with TOF-MS with data-independent acquisition has been developed. The limit of identification was evaluated for all 256 compounds and 95 of these compounds were validated with regard to matrix effects, extraction recovery, and process efficiency. The limit of identification ranged from 0.001 to 0.1 mg/kg, and the process efficiency exceeded 50% for 73 of the 95 analytes. As an example of application, 1335 forensic traffic cases were analyzed with the presented screening method. Of these, 992 cases (74%) were positive for one or more traffic-relevant drugs above the Danish legal limits. Commonly abused drugs such as amphetamine, cocaine, and frequent types of benzodiazepines were the major findings. Nineteen less frequently encountered drugs were detected e.g. buprenorphine, butylone, cathine, fentanyl, lysergic acid diethylamide, m-chlorophenylpiperazine, 3,4-methylenedioxypyrovalerone, mephedrone, 4-methylamphetamine, p-fluoroamphetamine, and p-methoxy-N-methylamphetamine. In conclusion, using UHPLC-TOF-MS screening with data-independent acquisition resulted in the detection of common drugs of abuse as well as new designer drugs and more rarely occurring drugs. Thus, TOF-MS screening of blood samples constitutes a practical way for screening traffic cases, with the exception of δ-9-tetrahydrocannabinol, which should be handled in a separate method.

Drugged driving arrests in Norway before and after the implementation of per se law

“…A large number of drugs can be included, since evidence regarding impairment is not requested. Denmark has fixed-concentration limits, and more than 200 substances are included in the screening analysis [39]. The penalty is loss of driving license and a fee.…”

High-resolution mass spectrometry in toxicology: current status and future perspectives

“…The LODs were at least 1 mg/kg blood, and all samples had to be injected twice: one time in positive and one time in negative ionization mode. The second procedure (Pedersen et al 2013) reported LODs typically below 0.1 mg/kg blood, and identification criteria were identical to those by Dalsgaard et al The analysis covered 256 compounds, but only for 95 compounds, matrix effect, extraction recovery, and process efficiency were studied. Most of the common DoA could be detected by this approach with the exception of delta-9-tetrahydrocannabinol.…”

“…The group of Linnet presented two screening procedures based on this data-independent principle: one optimizing a previously described system for screening of 30 acidic and neutral drugs in whole blood (Dalsgaard et al 2013) and one as broad forensic screening method in whole blood samples both after fully automated off-line SPE robotic extraction (Pedersen et al 2013). The first procedure identified compounds based on retention time (0.2 min window) and the presence of one fragment ion and/or isotopic pattern.…”

An overview of recent developments in the analytical detection of new psychoactive substances (NPSs)

“…The manuscript with its real and imaginative title, "Taking the Pissoira novel and reliable way of knowing what drugs are being used in nightclubs", reported the detection of classical recreational drugs and NPSs such as: mephedrone, 3′-trifluoromethylphenylpiperazine and 2-aminoindane using various chromatographic and mass spectrometric methods. 44 Earlier reports in Denmark, Pedersen et al 35 presented an automated solid-phase extraction (SPE) and ultra-highperformance liquid chromatography (UHPLC) with time of flight-mass spectrometry (TOF-MS) screening method for 256 illicit compounds in blood and 95 of these compounds were validated with regard to matrix effects, extraction recovery, and process efficiency with the limit of detection (LOD) ranging from 0.001 to 0.1 mg kg −1 . 19 In the same year, Leffler et al 44 (located in the United States) analysed 14 separate street samples wherein 10 synthetic cathinones were identified employing a variety of techniques, including gas chromatography with mass spectrometric detection (GC-MS) and flame ionization (GC-FID).…”