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Paper spray mass spectrometry is presented as a direct, quantitative tool for the measurement of pharmaceutical drugs and a variety of fentanyl analogs in solid samples and powder slurries with the ultimate goal of providing meaningful harm-reduction drug checking. Method development and validation was carried out for fentanyl analog slurries as a proxy for street drug samples. Lower limits of quantitation were determined to be 3.6-7.4 ng/g for fentanyl analogs in the pharmaceutical slurry matrix. Using 1mg of solid sample, the method can quantify picogram quantities of these drugs, well below required thresholds for even the most potent fentanyl analogs. Quality control samples were prepared and used to assess method validity according to the Scientific Working Group for Forensic Toxicology (SWGTOX) guidelines. Performance metrics for both precision and accuracy were found to be within SWGTOX-recommended guidelines. Additionally, pharmaceutical tablets were used to demonstrate the applicability of the developed paper spray methodology for the direct qualitative and quantitative analysis of active ingredients in pharmaceutical powders deposited directly onto the paper spray substrate. A proposed workflow for rapid solid drug sample measurements is presented with potential applications for point-of-use street drug measurements and other solid sample matrices. Natural Sciences and Engineering Research Council of Canada, Grant/Award Number: RGPIN-2016-05380 This article was originally published as: Borden, S.A., Saatchi, A., Krogh, E.T., & Gill, C.G. (2020). Rapid and quantitative determination of fentanyls and pharmaceuticals from powdered drug samples by paper spray mass spectrometry. Analytical Science Advances, 2(1), 97-108. https://doi.org/10.1002/ansa.202000083 Analytical Science Advances, an open-access journal published by Wiley-VCH, is available online at: https://onlinelibrary.wiley.com/journal/26285452. This article is licensed under a Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License. https://viurrspace.ca/bitstream/handle/10613/23357/KroghGill2020ANSA.pdf?sequence=3

Introduction. Drug checking services for harm reduction and overdose prevention have been implemented in many jurisdictions as a public health intervention in response to the opioid overdose crisis. This study demonstrates the first on-site use of paper spray mass spectrometry for quantitative drug checking to address the limitations of current on-site drug testing technologies. Methods. Paper spray mass spectrometry was used to provide on-site drug checking services at a supervised consumption site in the Downtown Eastside of Vancouver, British Columbia, Canada during a 2-day pilot test in August 2019. The method included the targeted quantitative measurement of 49 drugs and an untargeted full scan to assist in identifying unknown/unexpected components. Results. During the pilot, 113 samples were submitted for analysis, with 88 (78%) containing the client expected substance. Fentanyl was detected in 45 of 59 expected fentanyl samples, and in 50 (44%) samples overall at a median concentration of 3.6% (w/w%). The synthetic precursor of fentanyl, 4-anilino-N-phenethyl-piperidine (4-ANPP), was found in 74.0% of all fentanyl samples at a median concentration of 2.2%, suggesting widespread poor manufacturing practices. Etizolam was detected in 10 submitted samples anticipated to be fentanyl at a median concentration of 2.5%. No clients submitting these samples expected etizolam or a benzodiazepine in their sample. In three instances, it was co-measured with fentanyl, and in seven cases it was detected alone. Discussion and Conclusions. The quantitative capabilities and low detection limits demonstrated by paper spray mass spectrometry offer distinct benefits over existing on-site drug checking methods and harm reduction services.