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6 protocols using thccooh

1

Analytical Method for Cannabis Compounds

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THC, 11-OH-THC, THCCOOH, THCCOOH-gluc, CBD, CBN, d3-THC, d3-11-OH-THC, d9-THCCOOH, d3-CBD, d3-CBN and d3-THCCOOH-gluc (d3-THCCOOH-gluc) were purchased from Cerilliant (Round Rock, TX, USA). CBG was obtained from Restek (Bellefonte, PA, USA), THCAA was from Lipomed (Arlesheim, Switzerland), THCVCOOH and THC-gluc from ElSohly Laboratories (Oxford, MS, USA) and THCV from RTI International (Research Triangle Park, NC, USA). Acetonitrile, ammonium acetate and formic acid (LC-MS grade) were acquired from Sigma Aldrich (St. Louise, MO, USA) and methanol (LC-MS grade) from Fischer Scientific (Fair Lawn, NJ, USA). Water was purified in-house by an ELGA Purelab Ultra Analytic purifier (Siemens Water Technologies, Lowell, MA, USA). WAX-S tips (DPX Labs, Columbia, SC, USA) were used to extract samples, and a Kinetex C18 2.1 × 50 mm, 2.6 μm column combined with a 2.1 × 2 mm guard column of identical phase (Phenomenex Inc., Torrance, CA, USA) accomplished analyte separation.
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2

Quantitative Analysis of THC Compounds

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THC, THC-COOH, THC-OH, THC-D3, THC-COOH-D3, and THC-OH-D9 were purchased from Cerilliant (Round Rock, TX, USA). A second set of THC, THC-OH, and THC-COOH was purchased from Lipomed (Cambridge, MA, USA) to be used for quality control samples. Water and acetonitrile (LC–MS-grade) were obtained from Millipore (Burlington, MA, USA). Dansyl chloride, sodium bicarbonate, sodium carbonate, acetic acid, and formic acid (LC–MS-grade) were obtained from Sigma-Aldrich (St. Louis, MO, USA). Captiva EMR-Lipid columns (1 mL, 40 mg) were purchased from Agilent Technologies (Santa Clara, CA, USA). Chromatography was performed with a Kinetex Phenyl Hexyl column (3.0 × 50 mm, 2.6 μm) purchased from Phenomenex Inc. (Torrance, CA, USA).
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3

Comprehensive Cannabinoid Standard Preparation

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Stocks of 1 mg/mL of CBD, THC, CBN, 11-OH-THC, CBG, THCV, THCA-A, and THCCOOH-D 3 as well as 100 μg/mL solutions of THCCOOH, THCCOOH-gluc, CBD-D 3 , THC-D 3 , CBN-D 3 , and 11-OH-THC-D 3 were purchased from Cerilliant (Round Rock, TX, USA). A 10-μg/mL THCgluc stock was obtained from ElSohly (Oxford, MS, USA).
Optima LC/MS grade acetonitrile, methanol, 2-propanol, formic acid (FA), and ammonium acetate were obtained from Fisher Scientific (Hampton, NH, USA). Oasis PRiME HLB 96-well solid-phase extraction (SPE) plates with 30 mg sorbent/well, 96-well collection plates, quick-load glass inserts, silicone/PTFE-treated 96-well square plug cap mats, and amber max recovery autosampler vials were acquired from Waters (Milford, MA, USA). Borosilicate glass tubes were from Fisher Scientific and 18.2 MΩ-cm water was dispensed from a Siemens PureLab Ultra purification system.
Blank WB was created by mixing acid citrate dextrose (ACD)packed red blood cells with ABO-compatible plasma and confirming the absence of detectable cannabinoids. Breath matrix consisted of an unused SensAbues ® electret filter material ("pad") cut into 28 cm 2 squares to match the intake surface area of the SensAbues ® collection device.
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4

Quantitative Analysis of Cannabinoids

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THC, 11-OH-THC, THCCOOH, CBD, CBN, THC-d3, 11-OH-THC-d3, THCCOOH-d9, CBD-d3, CBN-d3, and THCCOOH-glucuronide-d3 were purchased from Cerilliant (Round Rock, TX, USA). CBG was from Restek (Bellefonte, PA, USA), THCV was from RTI International (Research Triangle Park, NC, USA), and THCVCOOH and THC-glucuronide were acquired from ElSohly Laboratories (Oxford, MS, USA). Ammonium acetate and acetonitrile (LC-MS grade) were obtained from Sigma-Aldrich (St. Louis, MO, USA). Methanol and water (LC-MS grade) and formic acid (ACS-grade) were from Fisher Scientific (Fair Lawn, NY, USA). WAX-S tips (1 mL tip containing 20 mg resin and 40 mg salt) were purchased from DPX Labs (Columbia, SC, USA). Chromatography was performed on a Kinetex® C18 column (Phenomenex® Inc., Torrance CA, USA; 2.1 mm × 50 mm, 2.6 μm) combined with a SecurityGuard™ C18 guard column (4 × 2.0 mm).
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5

Quantification of THCCOOH in Oral Fluid

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THCCOOH (1 mg/mL) and THCCOOH-d3 (100 mcg/mL) were purchased from Cerilliant Corporation (Round Rock, TX). Trifluoroacetic anhydride (TFAA) and hexafluoroisopropanol (HFIP) were supplied by Campbell Science (Rockton, IL). Acetone, acetonitrile, ethyl acetate, and hexane were purchased from Sigma-Aldrich (Milwaukee, WI), and ammonium hydroxide (28%–30%), glacial acetic acid, and methanol were from Mallinckrodt Baker (Phillipsburg, NJ). All chemicals and organic solvents were ACS reagent grade and high pressure liquid chromatography grade, respectively. A CEREX System 48 positive pressure manifold and CEREX Polychrom THC (3 mL/35 mg) extraction columns from SPEware Corporation (Baldwin Park, CA) were used for specimen extraction. Quantisal devices for the collection of oral fluid specimens and Quantisal transport buffer for diluting calibrator standards were obtained from Immunalysis Corporation (Pomona, CA). Oral-Eze devices and Oral-Eze transport buffer were obtained from Capital Vial, Inc (Auburn, AL).
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6

Quantitative Analysis of Cannabinoids

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THC, THC-OH, THC-COOH and CBD at 1 mg/mL, and THCCOOH-glucuronide and the internal standards (IStd) THC-d3, THC-OH-d3 and THCCOOH-d3 at 0.1 mg/mL in methanol were purchased from Cerilliant (Round Rock, TX, USA). THC-diOH and THC-diOH-d6 at 0.1 mg/mL and THC-glucuronide at 0.01 mg/mL in methanol were from ElSohly Laboratories (Oxford, MS, USA). Solid phase extraction (SPE) mixed-mode cation exchange cartridges (Strata Drug X-C, 3 mL, 60 mg) were purchased from Phenomenex (Torrance, CA, USA). Formic acid was obtained from Pharmco-Aaper (Shelbyville, KY, USA). Methanol, acetonitrile, dichloromethane, and isopropanol were acquired from Fisher Scientific (Pittsburgh, PA, USA). Solvents for the extraction were high performance liquid chromatography (HPLC) grade and for the chromatographic instrument were liquid chromatography-mass spectrometry (LC-MS) grade.
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