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A reliable and validated LC-MS/MS method for the simultaneous quantification of 4 cannabinoids in 40 consumer products.
PLoS One 2018; 13(5):e0196396Plos

Abstract

In the past 50 years, Cannabis sativa (C. sativa) has gone from a substance essentially prohibited worldwide to one that is gaining acceptance both culturally and legally in many countries for medicinal and recreational use. As additional jurisdictions legalize Cannabis products and the variety and complexity of these products surpass the classical dried plant material, appropriate methods for measuring the biologically active constituents is paramount to ensure safety and regulatory compliance. While there are numerous active compounds in C. sativa the primary cannabinoids of regulatory and safety concern are (-)-Δ⁹-tetrahydrocannabinol (THC), cannabidiol (CBD), and their respective acidic forms THCA-A and CBDA. Using the US Food and Drug Administration (FDA) bioanalytical method validation guidelines we developed a sensitive, selective, and accurate method for the simultaneous analysis CBD, CBDA, THC, and THCA-A in oils and THC & CBD in more complex matrices. This HPLC-MS/MS method was simple and reliable using standard sample dilution and homogenization, an isocratic chromatographic separation, and a triple quadrupole mass spectrometer. The lower limit of quantification (LLOQ) for analytes was 0.195 ng/mL over a 0.195-50.0 ng/mL range of quantification with a coefficient of correlation of >0.99. Average intra-day and inter-day accuracies were 94.2-112.7% and 97.2-110.9%, respectively. This method was used to quantify CBD, CBDA, THC, and THCA-A in 40 commercial hemp products representing a variety of matrices including oils, plant materials, and creams/cosmetics. All products tested met the federal regulatory restrictions on THC content in Canada (<10 μg/g) except two, with concentrations of 337 and 10.01 μg/g. With respect to CBD, the majority of analyzed products contained low CBD levels and a CBD: CBDA ratio of <1.0. In contrast, one product contained 8,410 μg/g CBD and a CBD: CBDA ratio of >1,000 (an oil-based product). Overall, the method proved amenable to the analysis of various commercial products including oils, creams, and plant material and may be diagnostically indicative of adulteration with non-hemp C. sativa, specialized hemp cultivars, or unique manufacturing methods.

Authors+Show Affiliations

Research and Development, Delivra Corp., Charlottetown, PE, Canada.Research and Development, Delivra Corp., Charlottetown, PE, Canada.Research and Development, Delivra Corp., Charlottetown, PE, Canada.Research and Development, Delivra Corp., Charlottetown, PE, Canada.Research and Development, Delivra Corp., Charlottetown, PE, Canada.Research and Development, Delivra Corp., Charlottetown, PE, Canada.

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't
Validation Studies

Language

eng

PubMed ID

29718956

Citation

Meng, Qingfang, et al. "A Reliable and Validated LC-MS/MS Method for the Simultaneous Quantification of 4 Cannabinoids in 40 Consumer Products." PloS One, vol. 13, no. 5, 2018, pp. e0196396.
Meng Q, Buchanan B, Zuccolo J, et al. A reliable and validated LC-MS/MS method for the simultaneous quantification of 4 cannabinoids in 40 consumer products. PLoS ONE. 2018;13(5):e0196396.
Meng, Q., Buchanan, B., Zuccolo, J., Poulin, M. M., Gabriele, J., & Baranowski, D. C. (2018). A reliable and validated LC-MS/MS method for the simultaneous quantification of 4 cannabinoids in 40 consumer products. PloS One, 13(5), pp. e0196396. doi:10.1371/journal.pone.0196396.
Meng Q, et al. A Reliable and Validated LC-MS/MS Method for the Simultaneous Quantification of 4 Cannabinoids in 40 Consumer Products. PLoS ONE. 2018;13(5):e0196396. PubMed PMID: 29718956.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - A reliable and validated LC-MS/MS method for the simultaneous quantification of 4 cannabinoids in 40 consumer products. AU - Meng,Qingfang, AU - Buchanan,Beth, AU - Zuccolo,Jonathan, AU - Poulin,Mathieu-Marc, AU - Gabriele,Joseph, AU - Baranowski,David Charles, Y1 - 2018/05/02/ PY - 2017/12/20/received PY - 2018/04/12/accepted PY - 2018/5/3/entrez PY - 2018/5/3/pubmed PY - 2018/8/14/medline SP - e0196396 EP - e0196396 JF - PloS one JO - PLoS ONE VL - 13 IS - 5 N2 - In the past 50 years, Cannabis sativa (C. sativa) has gone from a substance essentially prohibited worldwide to one that is gaining acceptance both culturally and legally in many countries for medicinal and recreational use. As additional jurisdictions legalize Cannabis products and the variety and complexity of these products surpass the classical dried plant material, appropriate methods for measuring the biologically active constituents is paramount to ensure safety and regulatory compliance. While there are numerous active compounds in C. sativa the primary cannabinoids of regulatory and safety concern are (-)-Δ⁹-tetrahydrocannabinol (THC), cannabidiol (CBD), and their respective acidic forms THCA-A and CBDA. Using the US Food and Drug Administration (FDA) bioanalytical method validation guidelines we developed a sensitive, selective, and accurate method for the simultaneous analysis CBD, CBDA, THC, and THCA-A in oils and THC & CBD in more complex matrices. This HPLC-MS/MS method was simple and reliable using standard sample dilution and homogenization, an isocratic chromatographic separation, and a triple quadrupole mass spectrometer. The lower limit of quantification (LLOQ) for analytes was 0.195 ng/mL over a 0.195-50.0 ng/mL range of quantification with a coefficient of correlation of >0.99. Average intra-day and inter-day accuracies were 94.2-112.7% and 97.2-110.9%, respectively. This method was used to quantify CBD, CBDA, THC, and THCA-A in 40 commercial hemp products representing a variety of matrices including oils, plant materials, and creams/cosmetics. All products tested met the federal regulatory restrictions on THC content in Canada (<10 μg/g) except two, with concentrations of 337 and 10.01 μg/g. With respect to CBD, the majority of analyzed products contained low CBD levels and a CBD: CBDA ratio of <1.0. In contrast, one product contained 8,410 μg/g CBD and a CBD: CBDA ratio of >1,000 (an oil-based product). Overall, the method proved amenable to the analysis of various commercial products including oils, creams, and plant material and may be diagnostically indicative of adulteration with non-hemp C. sativa, specialized hemp cultivars, or unique manufacturing methods. SN - 1932-6203 UR - https://www.unboundmedicine.com/medline/citation/29718956/A_reliable_and_validated_LC_MS/MS_method_for_the_simultaneous_quantification_of_4_cannabinoids_in_40_consumer_products_ L2 - http://dx.plos.org/10.1371/journal.pone.0196396 DB - PRIME DP - Unbound Medicine ER -