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4 protocols using acrylfentanyl

1

Quantitative Analysis of Synthetic Opioids

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Standard of acetylfentanyl (hydrochloride), acrylfentanyl (hydrochloride), alfentanil (hydrochloride), butyrylfentanyl, carfentanyl, (±)-cis-3-methylfentanyl (hydrochloride), (±)-cis-3-methylthiofentanyl (hydrochloride), fentanyl (hydrochloride), furanylfentanyl (hydrochloride), α-methylfentanyl (hydrochloride), α-methylthiofentanyl (hydrochloride), β-hydroxyfentanyl (hydrochloride), ortho-fluorofentanyl (hydrochloride), ocfentanyl, para-fluorofentanyl (hydrochloride), remifentanyl (hydrochloride), sufentanyl, 4-ANPP, norfentanyl, butyrylfentanyl carboxy metabolite, despropionylpara-fluorofentanyl, (±)-trans-3-methyl norfentanyl, methoxyacetyl norfentanyl (hydrochloride), valerylfentanyl carboxy metabolite, morphine, methadone, EDDP, 6-MAM, codeine, MT-45, fentanyl-d5 (hydrochloride) and nordentanyl-d5 were purchased from Cayman Chemical (Ann Arbor, MI, USA) in form of methanolic solution at the concentration of 1 mg mL−1. Working solutions were prepared at the concentration of 1 μg mL−1 and stored at −20 °C. Water, methanol, acetonitrile and 2-propanol were obtained from Carlo Erba (Milano, Italia) while sodium carbonate, sodium bicarbonate and ammonium formate were purchased from Sigma-Aldrich (Milwaukee, WI, USA).
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2

Opioid and Synthetic Opioid Separations

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The run buffer used for opioid and synthetic opioid separations was 12 mmol/L acetic acid, 3.3 mmol/L ammonium acetate pH 4.4 (Sigma-Aldrich, St. Louis, MO, USA) in ultrapure water (Millipore Milli-Q, 18.0 MΩ-cm). Acetaminophen, caffeine, mannitol, procaine, quinine, and methanol were all purchased from Sigma-Aldrich (St. Louis, MO, USA).
All fentanyl analogues (acetyl fentanyl, acryl fentanyl, benzyl fentanyl, butyryl fentanyl, furanyl fentanyl, methacryl fentanyl, methoxyacetyl fentanyl, phenyl fentanyl, valeryl fentanyl) were purchased as hydrochloride salts from Cayman Chemical (Ann Arbor, MI, USA) or, when possible, as 1 mg·mL−1 methanolic solutions. Powdered standards and samples were dissolved gravimetrically in methanol (Sigma-Aldrich, St. Louis, MO). The remaining opioids and narcotics (heroin, fentanyl, cocaine, U-47700) were purchased as 1 mg·mL−1 solutions in methanol or acetonitrile from Cerilliant (Round Rock, TX, USA). All sample dilutions were prepared in run buffer, and methanol was added as necessary to allow for a constant 4 % by volume organic solvent across all analyses. When increased analyte concentrations were desired, standards were concentrated to assure each sample contained a maximum of 4 % (v/v) solvent.
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3

Quantification of Novel Fentanyl Analogs

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Acetylfentanyl, acrylfentanyl, furanylfentanyl and 4-fluoro-isobutyrylfentanyl were purchased as powders from Cayman Chemical (Ann Arbor, USA), diclofenac from Sigma (Stockholm, Sweden). Cryopreserved hepatocytes LiverPool (10-donor-pool), InVitro Gro HT and InVitro Gro KHB media were obtained from Bioreclamation IVT (Brussels, Belgium). Liquid chromatography mass spectrometry grade acetonitrile, water, methanol and formic acid were from Fisher Scientific (Gothenburg, Sweden), ammonium formate from Fluka (Sigma-Aldrich, Stockholm, Sweden), ammonium acetate and acetic acid from Merck (Darmstadt, Germany). The βglucuronidase/sulfatase mixture (Helix pomatia) was purchased from Roche (Mannheim, Germany). Ultra-pure water was prepared in-house using a MilliQ Gradient 10 production unit (Millipore, Billerica, USA).
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4

Sourcing and Characterization of Fentanyl Analogues

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Fentanyl, 4-ANPP, Valeryl Fentanyl, Furanyl Fentanyl, Methoxyacetyl Fentanyl, Acetyl Fentanyl, Acryl Fentanyl, and 2′-fluoro ortho-FluoroFentanyl were purchased from Cayman Chemical Company (Ann Arbor, MI). Perchloric acid was obtained from Fisher Scientific (Fair Lawn, NJ). Potassium chloride was received from Sigma-Aldrich (St. Louis, MO). Water (18.2 MΩ) was obtained using a Millipore Direct-Q ® UV water purification system (Billerica, MA).
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