title: Analysis of new designer drugs in post-mortem blood using high-resolution mass spectrometry.
abstract: An analytical method was developed and validated for the purpose of detecting and quantifying 37 new designer drugs including cathinones, hallucinogenic phenethylamines and piperazines. Using only 100 µL whole blood, a salting-out-assisted liquid-liquid extraction with acetonitrile was performed to isolate target compounds followed by chromatographic separation using a Waters ACQUITY ultra performance liquid chromatograph coupled to a Waters XEVO quadrupole time-of-flight mass spectrometer. Mephedrone-d3 was used as an internal standard. A gradient elution was used in combination with a Waters ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 µm). Samples were analyzed using the detector in positive electrospray ionization mode with MS(E) acquisition. All compounds of interest were resolved in a 15 min run time and positively identified based on accurate mass of the molecular ion, two product ions and retention time. All analyte calibration curves were linear over the range of 0.05-2 mg/L with most correlation coefficient (r(2)) values >0.98. The limits of detection were within the range of 0.007-0.07 mg/L and limits of quantification within 0.05-0.1 mg/L. All analytes were stable 48 h after extraction and most were stable in blood after 1 week stored in a refrigerator and 3 freeze-thaw cycles. No carryover was observed up to 10 mg/L and no interferences from common therapeutic drugs or endogenous compounds. Recoveries ranged from 71 to 100% and matrix effects were assessed for blank, post-mortem and decomposed blood. All bias and % coefficient of variation values were within the acceptable values of ±15 and ≤15%, respectively (±20 and ≤20% at lower limit of quantification). The method was applied to several forensic cases where the subject exhibited behavior characteristic of designer drug intoxication and where routine screening for a panel of drugs was negative.
authors.affiliation: Centre for Forensic Science, University of Technology Sydney (UTS), Broadway, NSW 2007, Australia daniel.pasin@student.uts.edu.au.
authors.forename: Daniel
authors.initials: D
authors.lastname: Pasin
authors.affiliation: Forensic Toxicology Laboratory, NSW Forensic and Analytical Science Service (FASS), Lidcombe, NSW 2141, Australia.
authors.forename: Sergei
authors.initials: S
authors.lastname: Bidny
authors.affiliation: Centre for Forensic Science, University of Technology Sydney (UTS), Broadway, NSW 2007, Australia.
authors.forename: Shanlin
authors.initials: S
authors.lastname: Fu
mesh_terms: D000328:Adult; D000818:Animals; D001344:Autopsy; D002138:Calibration; D002423:Cause of Death; D002851:Chromatography, High Pressure Liquid; D015198:Designer Drugs / Q000032:analysis*; D004355:Drug Stability; D053593:Forensic Toxicology / Q000379:methods* / Q000592:standards; D006801:Humans; D057230:Limit of Detection; D016014:Linear Models; D059625:Liquid-Liquid Extraction; D008297:Male; D011237:Predictive Value of Tests; D012015:Reference Standards; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000592:standards; D015813:Substance Abuse Detection / Q000379:methods* / Q000592:standards; D019966:Substance-Related Disorders / Q000097:blood* / Q000175:diagnosis / Q000401:mortality; D034421:Sus scrofa
chemical_list: D015198:Designer Drugs