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.
PurposeThe 4-chloromethcathinone (4-CMC) is a synthetic derivative of cathinone and belongs to new psychoactive substances. Neither data on the effects of 4-CMC on the human body, nor on nontoxic, toxic and lethal concentrations in biological materials have been published in the literature. This paper describes the results of an analysis of the blood concentrations of 4-CMC determined in 15 forensic cases related to nonfatal intoxication including driving under the influence, and fatalities including overdoses, suicide and traffic accidents.MethodsA new method for the quantification of 4-CMC using gas chromatography–mass spectrometry (GC–MS) was developed. The symptoms of 4-CMC use were also studied based on an analysis of the documents prepared during the collection of samples or at autopsies.ResultsThe limits of detection and quantification of the method for blood samples were 0.3 and 1 ng/mL, respectively. The calibration curve was linear in the studied concentration range (1–500 ng/mL) with the correlation coefficient at 0.9979. The extraction recoveries varied in the range of 94.3–98.8%. The accuracy and precision were acceptable. The determined concentrations in nonfatal cases ranged from 1.3 to 75.3 ng/mL, and in fatalities from 56.2 to 1870 ng/mL.ConclusionsOur study can assist in the recognition of the possible effects caused by 4-CMC and can be helpful during the preparation of forensic toxicological opinions for courts of law. The validation parameters indicate the sensitivity and accuracy of the method. This is the first work presenting a validated method for the determination of 4-CMC in blood samples by GC–MS.
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.
MDPBP (1-(3,4-methylenedioxyphenyl)-2-(1-pyrrolidinyl)-1-butanone) is a new psychoactive substance sold on the black market. It has been a controlled drug of abuse in Poland and China since 2015 as some toxic and fatal cases connected with use of synthetic cathinone derivatives were observed. The fatal case outlined here concerns a 19-year-old man, who was found dead with an envelope containing white powder lying nearby the cadaver. The analyses of the powder revealed a presence of MDPBP. Due to this, blood was tested for routine toxicological analysis for traditional drugs and for MDPBP by liquid–liquid extraction procedure with 1-chlorobutane followed by GC–MS analysis. Full validation of proposed method was performed. Limit of detection and limit of quantification were 10.1 and 30.4 ng/cm3, respectively. Calibration curve was linear in studied concentration range (25–1000 ng/cm3) with a correlation coefficient 0.9946. The trueness and inter-day precision expressed as recoveries and CV values were investigated at 3 concentrations: 25, 250, and 1000 ng/cm3. The CV values were less than 20 % in the lowest concentration and less than 15 % in other concentrations what met the internationally established acceptance criteria for bioanalytical methods. It indicates good precision and accuracy of the method. The analysis of blood sample showed very high concentration of MDPBP (9.32 µg/cm3), which suggests possibility of overdosing. To the best of our knowledge, this is the first work which presents determination of MDPBP in blood by GC-EI-MS method and the third fatal accident report of MDPBP abuse.Graphical abstract
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