Characterization of fentanyl HCl powder prior to and after systematic degradation.

Fentanyl HCl is of particular interest in forensic cases but there is a notable gap in literature regarding its analysis. This study utilized a multi-method approach to characterize fentanyl HCl powder, both fresh and following a forced degradation process. Using sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) and direct injection gas chromatography-mass spectrometry (GC-MS), five compounds were identified in fresh fentanyl HCl powder. The identified compounds were: N-phenylpropanamide, 1-phenethyl-4-propionyloxypiperidine (1-P-4-POP), 4-anilino-N-phenethylpiperidine (4-ANPP), acetylfentanyl, and fentanyl; all identified compounds but acetylfentanyl and fentanyl decreased in quantity as the sample was degraded. Fresh headspace samples analyzed with solid phase microextraction (SPME)-GC-MS identified four compounds in common with the powder analyses: N-phenylpropanamide,1-P-4-POP, 4-ANPP, and fentanyl. Acetylfentanyl was not present in the headspace samples, although two additional compounds were: N-phenylacetamide and N-phenethyl-4-piperidinone (NPP). Where direct analysis of degraded fentanyl HCl showed decreased quantities of the identified compounds, headspace samples of the degraded fentanyl HCl resulted in higher quantities, implying that the degradation process drove those compounds to volatilize. Notably, fentanyl was identified in the headspace, implying that this could be an appropriate target for standoff detection. Finally, thermogravimetric analysis (TGA) and differential scanning calorimetry (DCS) confirmed that the forced degradation process had little permanent effect on the powder.

An optimized method for sample collection, extraction, and analysis of fentanyl and fentanyl analogs from a non-porous surface.

Illicit use of the potent opioid fentanyl and its analogs (fentanyls) are on the rise in the United States. As use increases, drug production tends to also increase, leading to more locations being contaminated with the potentially lethal substance. Because fentanyl-contaminated locations may present a risk to the general public, a method for sampling, identifying, and quantitating these fentanyls from surfaces is in need. This research developed and optimized a surface-wipe collection and extraction method for 17 fentanyls and 10 common fentanyl adulterants from a non-porous surface and quantitated the amount of each compound collected with liquid chromatography tandem mass spectrometry. The final, optimized surface-wipe method resulted in an average collection and extraction efficiency (±SD) of 62.0 (±14.0)%, with a range of 34.1 (±2.6) - 82.5 (±9.6)%. While legislation has yet to be implemented regarding remediation levels for fentanyl-contaminated locations, when such legislation is drafted, this method can be implemented to determine the safety of these locations prior to and after decontamination has occurred.

Estimating drug consumption during a college sporting event from wastewater using liquid chromatography mass spectrometry.

Consumption of licit and/or illicit compounds during sporting events has traditionally been monitored using population surveys, medical records, and law enforcement seizure data. This pilot study evaluated the temporal and geospatial patterns in drug consumption during a university football game from wastewater using liquid chromatography tandem mass spectrometry (LC-MS/MS). Untreated wastewater samples were collected from three locations within or near the same football stadium every 30 min during a university football game. This analysis leveraged two LCMS/ MS instruments (Waters Acquity TQD and a Shimadzu 8040) to analyze samples for 58 licit or illicit compounds and some of their metabolites. Bayesian multilevel models were implemented to estimate mass load and population-level drug consumption, while accounting for multiple instrument runs and concentrations censored at the lower limit of quantitation. Overall, 29 compounds were detected in at least one wastewater sample collected during the game. The 10 most common compounds included opioids, anorectics, stimulants, and decongestants. For compounds detected in more than 50% of samples, temporal trends in median mass load were correlated with the timing of the game; peak loads for cocaine and tramadol occurred during the first quarter of the game and for phentermine during the third quarter. Stadium-wide estimates of the number of doses of drugs consumed were rank ordered as follows: oxycodone (n = 3246) > hydrocodone (n = 2260) > phentermine (n = 513) > cocaine (n = 415) > amphetamine (n = 372) > tramadol (n = 360) > pseudoephedrine (n = 324). This analysis represents the most comprehensive assessment of drug consumption during a university football game and indicates that wastewater-based epidemiology has potential to inform public health interventions focused on reducing recreational drug consumption during large-scale sporting events.

Surface Contamination Generated by "One-Pot" Methamphetamine Production.

Methamphetamine production is the most common form of illicit drug manufacture in the United States. The "one-pot" method is the most prevalent methamphetamine synthesis method and is a modified Birch reduction, reducing pseudoephedrine with lithium and ammonia gas generated in situ. This research examined the amount of methamphetamine surface contamination generated by one-pot syntheses or "cooks", as well as the effectiveness of hosing with water as a simplified decontamination technique, to assess associated public health and environmental consequences. Concentrations of methamphetamine contamination were examined prior to production, after production, and after decontamination with water. Contamination was qualitatively field screened using lateral flow immunoassays and quantitatively assessed using a fluorescence covalent microbead immunosorbent assay. Following screening, 0 of 23 pre-cook samples, 29 of 41 post-cook samples, and 5 of 27 post-decontamination samples were positive. Quantitatively, one pre-cook sample had a methamphetamine concentration of 1.36 ng/100 cm2. Post-cook and post-decontamination samples had average methamphetamine concentrations of 26.50 ± 63.83 and 6.22 ± 12.17 ng/100 cm2, respectively. While all one-pot methamphetamine laboratories generate different amounts of waste, depending on the amount of precursors used and whether the reaction vessel remained uncompromised, this study examined the surface contamination generated by a popular one-pot method known to law enforcement. By understanding the amount of surface contamination generated by common methods of one-pot methamphetamine production and the effectiveness of decontamination techniques used to remediate them, health risks associated with these production sites can be better understood and environmental contamination can be mitigated.