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¹H NMR and HPLC/DAD for Cannabis sativa L. chemotype distinction, extract profiling and specification.
Talanta 2015; 140:150-165T

Abstract

The medicinal use of different chemovars and extracts of Cannabis sativa L. requires standardization beyond ∆9-tetrahydrocannabinol (THC) with complementing methods. We investigated the suitability of (1)H NMR key signals for distinction of four chemotypes measured in deuterated dimethylsulfoxide together with two new validated HPLC/DAD methods used for identification and extract profiling based on the main pattern of cannabinoids and other phenolics alongside the assayed content of THC, cannabidiol (CBD), cannabigerol (CBG) their acidic counterparts (THCA, CBDA, CBGA), cannabinol (CBN) and cannflavin A and B. Effects on cell viability (MTT assay, HeLa) were tested. The dominant cannabinoid pairs allowed chemotype recognition via assignment of selective proton signals and via HPLC even in cannabinoid-low extracts from the THC, CBD and CBG type. Substantial concentrations of cannabinoid acids in non-heated extracts suggest their consideration for total values in chemotype distinction and specifications of herbal drugs and extracts. Cannflavin A/B are extracted and detected together with cannabinoids but always subordinated, while other phenolics can be accumulated via fractionation and detected in a wide fingerprint but may equally serve as qualitative marker only. Cell viability reduction in HeLa was more determined by the total cannabinoid content than by the specific cannabinoid profile. Therefore the analysis and labeling of total cannabinoids together with the content of THC and 2-4 lead cannabinoids are considered essential. The suitability of analytical methods and the range of compound groups summarized in group and ratio markers are discussed regarding plant classification and pharmaceutical specification.

Authors+Show Affiliations

Centre for Pharmacognosy and Phytotherapy, Department for Pharmaceutical and Biological Chemistry, The School of Pharmacy, University College London, 29-39 Brunswick Square, London WC1N 1AX, United Kingdom. Electronic address: wieland.peschel@ema.europa.eu.Centre for Pharmacognosy and Phytotherapy, Department for Pharmaceutical and Biological Chemistry, The School of Pharmacy, University College London, 29-39 Brunswick Square, London WC1N 1AX, United Kingdom.

Pub Type(s)

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

Language

eng

PubMed ID

26048837

Citation

Peschel, Wieland, and Matteo Politi. "¹H NMR and HPLC/DAD for Cannabis Sativa L. Chemotype Distinction, Extract Profiling and Specification." Talanta, vol. 140, 2015, pp. 150-165.
Peschel W, Politi M. ¹H NMR and HPLC/DAD for Cannabis sativa L. chemotype distinction, extract profiling and specification. Talanta. 2015;140:150-165.
Peschel, W., & Politi, M. (2015). ¹H NMR and HPLC/DAD for Cannabis sativa L. chemotype distinction, extract profiling and specification. Talanta, 140, pp. 150-165. doi:10.1016/j.talanta.2015.02.040.
Peschel W, Politi M. ¹H NMR and HPLC/DAD for Cannabis Sativa L. Chemotype Distinction, Extract Profiling and Specification. Talanta. 2015 Aug 1;140:150-165. PubMed PMID: 26048837.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - ¹H NMR and HPLC/DAD for Cannabis sativa L. chemotype distinction, extract profiling and specification. AU - Peschel,Wieland, AU - Politi,Matteo, Y1 - 2015/03/05/ PY - 2014/09/20/received PY - 2015/02/12/revised PY - 2015/02/23/accepted PY - 2015/6/7/entrez PY - 2015/6/7/pubmed PY - 2016/3/2/medline KW - (1)H NMR KW - Analytical markers KW - CBD KW - CBG KW - Cannabis sativa L. KW - Extracts KW - HPLC KW - THC SP - 150 EP - 165 JF - Talanta JO - Talanta VL - 140 N2 - The medicinal use of different chemovars and extracts of Cannabis sativa L. requires standardization beyond ∆9-tetrahydrocannabinol (THC) with complementing methods. We investigated the suitability of (1)H NMR key signals for distinction of four chemotypes measured in deuterated dimethylsulfoxide together with two new validated HPLC/DAD methods used for identification and extract profiling based on the main pattern of cannabinoids and other phenolics alongside the assayed content of THC, cannabidiol (CBD), cannabigerol (CBG) their acidic counterparts (THCA, CBDA, CBGA), cannabinol (CBN) and cannflavin A and B. Effects on cell viability (MTT assay, HeLa) were tested. The dominant cannabinoid pairs allowed chemotype recognition via assignment of selective proton signals and via HPLC even in cannabinoid-low extracts from the THC, CBD and CBG type. Substantial concentrations of cannabinoid acids in non-heated extracts suggest their consideration for total values in chemotype distinction and specifications of herbal drugs and extracts. Cannflavin A/B are extracted and detected together with cannabinoids but always subordinated, while other phenolics can be accumulated via fractionation and detected in a wide fingerprint but may equally serve as qualitative marker only. Cell viability reduction in HeLa was more determined by the total cannabinoid content than by the specific cannabinoid profile. Therefore the analysis and labeling of total cannabinoids together with the content of THC and 2-4 lead cannabinoids are considered essential. The suitability of analytical methods and the range of compound groups summarized in group and ratio markers are discussed regarding plant classification and pharmaceutical specification. SN - 1873-3573 UR - https://www.unboundmedicine.com/medline/citation/26048837/¹H_NMR_and_HPLC/DAD_for_Cannabis_sativa_L__chemotype_distinction_extract_profiling_and_specification_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0039-9140(15)00122-8 DB - PRIME DP - Unbound Medicine ER -