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Potency testing of up to twenty cannabinoids by liquid chromatography diode array detector with optional electrospray ionization time-of-flight mass spectrometry.
Anal Chim Acta. 2022 May 15; 1207:339827.AC

Abstract

The growing popularity of Cannabis sativa L. and its widespread use for medical and recreational purposes have created an urgent demand of accurate and reliable analytical methods to identify and quantify a growing number of cannabinoids. To meet this demand, a liquid chromatography diode array detector (LC-DAD) method has been developed, validated, and applied in analysis of cannabinoids in nine samples of plant materials of marijuana, six samples of marijuana cigarettes, five samples of hemp flowers, one sample of hemp cigarette, and two samples of Δ8-tetrahydrocannabinol (Δ8-THC) fortified hemp flowers. The method has achieved significant improvements over published methods, which was characterized of 20 targeted cannabinoids, 18 quantified cannabinoids, baseline resolution among quantified cannabinoids, a low limit of quantification (0.02 μg mL-1), a wide linear range (0.02-25 μg mL-1 or 0.04-50% (w/w)), a unique experiment to track the recovery of sample preparation in real time by spiking abnormal cannabidiol (CBD), and a well-assessed specificity by electrospray ionization time-of-flight mass spectrometry (ESI/TOFMS). Precision and accuracy were assessed using quality control (QC) samples at three concentration levels, i.e., 0.02, 0.5, and 12.5 μg mL-1, in triplicates with inter-day and intra-day precision of less than 15% relative standard deviation (RSD) and accuracy of less than ±15% relative error, therefore meeting the requirements by the ISO 17025 standards. Additionally, ESI/TOFMS has discovered seven unknown cannabinoids, including one structural isomer of cannabigerol (CBG), one structural isomer of cannabinolic acid (CBNA), four structural isomers of Δ9-THC, and one structural isomer of Δ9-THC acetate. Furthermore, it uncovered that one of the two samples of Δ8-THC fortified hemp flowers contained 5.16% (w/w) Δ9-THC, an alarm to the current Δ8-THC craze by the public.

Authors+Show Affiliations

Department of Chemistry, Western Illinois University, Macomb, IL, 61455, USA. Electronic address: l-song@wiu.edu.Department of Chemistry, Western Illinois University, Macomb, IL, 61455, USA.Department of Chemistry, Western Illinois University, Macomb, IL, 61455, USA.Department of Chemistry, Western Illinois University, Macomb, IL, 61455, USA.Department of Chemistry, Western Illinois University, Macomb, IL, 61455, USA.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

35491034

Citation

Song, Liguo, et al. "Potency Testing of Up to Twenty Cannabinoids By Liquid Chromatography Diode Array Detector With Optional Electrospray Ionization Time-of-flight Mass Spectrometry." Analytica Chimica Acta, vol. 1207, 2022, p. 339827.
Song L, Valenzuela G, Carlson S, et al. Potency testing of up to twenty cannabinoids by liquid chromatography diode array detector with optional electrospray ionization time-of-flight mass spectrometry. Anal Chim Acta. 2022;1207:339827.
Song, L., Valenzuela, G., Carlson, S., Dodson, Z., & Adisa, M. (2022). Potency testing of up to twenty cannabinoids by liquid chromatography diode array detector with optional electrospray ionization time-of-flight mass spectrometry. Analytica Chimica Acta, 1207, 339827. https://doi.org/10.1016/j.aca.2022.339827
Song L, et al. Potency Testing of Up to Twenty Cannabinoids By Liquid Chromatography Diode Array Detector With Optional Electrospray Ionization Time-of-flight Mass Spectrometry. Anal Chim Acta. 2022 May 15;1207:339827. PubMed PMID: 35491034.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Potency testing of up to twenty cannabinoids by liquid chromatography diode array detector with optional electrospray ionization time-of-flight mass spectrometry. AU - Song,Liguo, AU - Valenzuela,Gabrielle, AU - Carlson,Shelby, AU - Dodson,Zachary, AU - Adisa,Mojisola, Y1 - 2022/04/11/ PY - 2022/02/12/received PY - 2022/04/02/revised PY - 2022/04/09/accepted PY - 2022/5/1/entrez PY - 2022/5/2/pubmed PY - 2022/5/4/medline KW - Cannabinoid KW - Diode array detector KW - Hemp KW - Liquid chromatography KW - Marijuana KW - Mass spectrometry SP - 339827 EP - 339827 JF - Analytica chimica acta JO - Anal Chim Acta VL - 1207 N2 - The growing popularity of Cannabis sativa L. and its widespread use for medical and recreational purposes have created an urgent demand of accurate and reliable analytical methods to identify and quantify a growing number of cannabinoids. To meet this demand, a liquid chromatography diode array detector (LC-DAD) method has been developed, validated, and applied in analysis of cannabinoids in nine samples of plant materials of marijuana, six samples of marijuana cigarettes, five samples of hemp flowers, one sample of hemp cigarette, and two samples of Δ8-tetrahydrocannabinol (Δ8-THC) fortified hemp flowers. The method has achieved significant improvements over published methods, which was characterized of 20 targeted cannabinoids, 18 quantified cannabinoids, baseline resolution among quantified cannabinoids, a low limit of quantification (0.02 μg mL-1), a wide linear range (0.02-25 μg mL-1 or 0.04-50% (w/w)), a unique experiment to track the recovery of sample preparation in real time by spiking abnormal cannabidiol (CBD), and a well-assessed specificity by electrospray ionization time-of-flight mass spectrometry (ESI/TOFMS). Precision and accuracy were assessed using quality control (QC) samples at three concentration levels, i.e., 0.02, 0.5, and 12.5 μg mL-1, in triplicates with inter-day and intra-day precision of less than 15% relative standard deviation (RSD) and accuracy of less than ±15% relative error, therefore meeting the requirements by the ISO 17025 standards. Additionally, ESI/TOFMS has discovered seven unknown cannabinoids, including one structural isomer of cannabigerol (CBG), one structural isomer of cannabinolic acid (CBNA), four structural isomers of Δ9-THC, and one structural isomer of Δ9-THC acetate. Furthermore, it uncovered that one of the two samples of Δ8-THC fortified hemp flowers contained 5.16% (w/w) Δ9-THC, an alarm to the current Δ8-THC craze by the public. SN - 1873-4324 UR - https://www.unboundmedicine.com/medline/citation/35491034/Potency_testing_of_up_to_twenty_cannabinoids_by_liquid_chromatography_diode_array_detector_with_optional_electrospray_ionization_time_of_flight_mass_spectrometry_ DB - PRIME DP - Unbound Medicine ER -