Purpose Psychoactive compounds that contain a phenylethylamine structure (such as amphetamine-type stimulants and synthetic cathinones) are one of the major classes of stimulants on the recreational drug market. Approximately 670 new psychoactive substances (NPS) are monitored only in Europe; however, new psychoactive compounds are being developed for illicit trade each year. In this context, the development of new analytical procedures for the determination of such compounds in biological specimens for forensic toxicology is of great importance. Methods Gas chromatography-tandem mass spectrometry (GC-MS/MS) technique was applied for analysis of amphetamines and synthetic cathinones. The volumes of 200 µL of each whole blood sample and 1 mL of liquid-liquid extraction solvent were used for extraction, followed by pentafluoropropionyl derivatization. Results A high-throughput, robust, rapid, and sensitive procedure involving a simple liquid-liquid extraction for the simultaneous determination of 45 amphetamine-type stimulants and synthetic cathinones in whole blood was developed. The assay was validated based on its recovery (83.2-106%), interday accuracy (89.0-108%), and interday precision (≤ 8.1%). In view of the low limits of detection (ranged between 0.02 and 0.72 ng/mL) and limits of quantification (1 and 2.5 ng/mL), the developed method can serve as a less expensive and more ecologically friendly alternative to the liquid chromatography-tandem mass spectrometric methods. Conclusions To the best of our knowledge, this is the first work presenting a GC-MS/MS method for the determination of NPS in blood samples. The presented procedure was applied to authentic samples from forensic cases, demonstrating its utility in the quantification of a wide number of psychoactive substances in routine toxicological analyses. The developed procedure can also be easily expanded to additional compounds. Keywords Amphetamine-type stimulants (ATSs) • Synthetic cathinones • Whole blood • GC-MS/MS Prof. Jacek Namieśnik passed away on 14 April 2019. He will always remain in our memory.
N-Ethylhexedrone [2-(ethyloamino)-1-phenylhexan-1-one; α-ethylaminohexanophenone; NEH] is one of the most recent synthetic cathinones that appeared on the illegal market in late 2015. The majority of information concerning the model of consumption of NEH and its impact on the body originates only from self-reports from grey literature websites and drug forums. There are only limited data associated with the concentrations of NEH in blood samples available in the literature. This article presents a case of fatal NEH intoxication and a method for the determination of this substance in whole blood. A 21-year-old man without any diagnosed diseases was admitted to the hospital due to disorientation, aggression and finally loss of consciousness. Hyperthermia (>41°C), tachycardia (>160 beats per minute), tachypnoe (20 breaths per minute), blood pressure (110/60 mmHg) and acute kidney failure were diagnosed. After a few hours of hospitalization, the patient died. A plastic bag with a white powder was found in his underwear. Analysis of the powder by another laboratory revealed cocaine hydrochloride; however, no cocaine or its metabolites were found in the biological material upon testing in our laboratory. Therefore, re-analysis of the powder was performed, and NEH was identified. Liquid-liquid extraction followed by LC–MS-MS analysis were used for the determination of NEH in blood. The validation parameters were as follows: calibration range 1–250 ng/mL, accuracy 106.5–109.9%, precision 3.5–6.3%, recovery 90.1–96.9%, LOD 0.07 ng/mL and LOQ 1 ng/mL. NEH was quantified in the blood at a concentration of 145 ng/mL. Additionally, amphetamine at low concentrations and THC-COOH were detected. Our study provided information on the possible lethal concentration and toxidrome that clinicians can observe for NEH-intoxicated patients and can be helpful during the preparation of toxicology analysis reports for a court of law for proper data interpretation.
Alcohol consumption during pregnancy constitutes one of the leading preventable causes of birth defects and neurodevelopmental disorders in the exposed children. Fatty acid ethyl esters (FAEEs), ethyl glucuronide (EtG) and ethyl sulfate (EtS) have been studied as potential biomarkers of alcohol consumption. However, most analytical approaches proposed for their analysis in meconium samples consist of separated extraction procedures requiring the use of two meconium aliquots, which is costly in terms of both time and materials. Therefore, the aim of this study was to develop and validate a method for the simultaneous extraction of 9 FAEEs, EtG and EtS from one meconium aliquot. The sample was homogenized using methanol, and then FAEEs were extracted with hexane while EtG and EtS were isolated using acetonitrile. Then, extracts were applied to solid-phase extraction columns and analysed by gas chromatography mass spectrometry (FAEEs) and liquid chromatography tandem mass spectrometry (EtG and EtS). Calibration curves were linear with r values greater than 0.99. The LODs ranged from 0.8 to 7.5 ng/g for FAEEs and were 0.2 ng/g and 0.8 ng/g for EtS and EtG, respectively. LOQs ranged from 5 to 25 ng/g for FAEEs and were 1 ng/g and 2.5 ng/g for EtS and EtG, respectively. Accuracies and precisions were between 93.8 and 107% and between 3.5 and 9.7%, respectively. The recovery values ranged from 89.1 to 109%. The method proved to be sensitive, specific, simple and fast and allowed for the reduction of the amount of organic solvent used for extraction compared to other published data while higher recoveries were obtained. The method was used for analysis of meconium samples in two cases of mothers who were consuming alcohol during pregnancy.
Benzodiazepines (BZDs) and Z-drugs are among the most commonly prescribed pharmaceuticals in the world and are considered standard care for various mental illnesses and for treatment of sleeping and anxiety disorders, alcohol withdrawal, muscle spasms and epilepsy. Some BZDs are not allowed as pharmaceuticals in many countries, and they are used as “designer benzodiazepines” (DBZDs). All these compounds are typically screened in routine toxicological analyses for forensic purposes. Knowledge of time-dependent decreases in drug concentrations during storage or transport of samples is of considerable significance and allows forensic toxicologists to achieve reliable data, proper interpretation and high-quality results. The aim of this study was to evaluate changes in the amounts of selected BZDs, DBZDs and Z-drugs in blood samples stored at various temperatures. The study involved BZDs (19), DBZDs (3) and Z-drugs (2) spiked into blank blood. Subsequently, the blood samples were stored at various temperatures (room temperature, 4°C, -20°C and -80°C) for up to six months. Analyses were performed at 1–2 week intervals using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The stability of compounds were evaluated under four temperature conditions over a 6 month. Some benzodiazepines were stable at all temperatures tested (e.g., diazepam, oxazepam, nordazepam, prazepam) and degradated of only 0-10%. The highest instability was observed for analyte samples kept at room temperature, and the losses in content for some compounds, e.g., lorazepam and chlordiazepoxide, were almost 100%. For other compounds, the stability was clearly different at each tested temperature. To the best of our knowledge, this is one of the first such comprehensive study of the long-term stability of benzodiazepines covering a wide range of different storage temperatures.
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