Dataset Information

Identification and quantification of cannabinol as a biomarker for local hemp retting in an ancient sedimentary record by HPTLC-ESI-MS.

ABSTRACT: Cannabis products have been used in various fields of everyday life for many centuries, and applications in folk medicine and textile production have been well-known for many centuries. For traditional textile production, hemp fibers were extracted from the stems by water retting in stagnant or slow-moving waters. During this procedure, parts of the plant material' among them phytocannabinoids' are released into the water. Cannabinol (CBN) is an important degradation product of the predominant phytocannabinoids found in Cannabis species. Thus, it is an excellent indicator for present as well as ancient hemp water retting. In this study, we developed and validated a simple and fast method for the determination of CBN in sediment samples using high-performance thin-layer chromatography (HPTLC) combined with electrospray ionization mass spectrometry (ESI-MS), thereby testing different extraction and cleanup procedures' as well as various sorbents and solvents for planar chromatography. This method shows a satisfactory overall analytical performance with an average recovery rate of 73%. Our protocol enabled qualitative and quantitative analyses of CBN in samples of a bottom sediment core' having been obtained from a small lake in Northern India, where intense local retting of hemp was suggested in the past. The analyses showed a maximum CBN content in pollen zone 4 covering a depth range of 262-209 cm, dating from approximately 480 BCE to 1050 CE. These findings correlate with existing records of Cannabis-type pollen. Thus, the method we propose is a helpful tool to track ancient hemp retting activities. Graphical Abstract.

SUBMITTER: Schmidt T

PROVIDER: S-EPMC7136313 | biostudies-literature | 2020 Apr

REPOSITORIES: biostudies-literature

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Identification and quantification of cannabinol as a biomarker for local hemp retting in an ancient sedimentary record by HPTLC-ESI-MS.

Schmidt Theresa T Kramell Annemarie Elisabeth AE Oehler Florian F Kluge Ralph R Demske Dieter D Tarasov Pavel E PE Csuk René R

Analytical and bioanalytical chemistry 20200214 11

Cannabis products have been used in various fields of everyday life for many centuries, and applications in folk medicine and textile production have been well-known for many centuries. For traditional textile production, hemp fibers were extracted from the stems by water retting in stagnant or slow-moving waters. During this procedure, parts of the plant material' among them phytocannabinoids' are released into the water. Cannabinol (CBN) is an important degradation product of the predominant p ...[more]

PMID: 32060580

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Project description:The objective of the present work was to develop a simple, specific, and fast high-performance thin-layer chromatographic (HPTLC) method to identify and quantify cordifolioside A, 20-β-hydroxyecdysone and columbin with HPTLC‒electrospray ionization‒tandem mass spectrometry (ESI‒MS/MS) for characterization in Tinospora cordifolia stem extracts. Chromatographic development was performed using a HPTLC aluminum plate, pre-coated with silica gel 60 F254 with hexane‒chloroform‒methanol‒formic acid as the mobile phase. Densitometric quantification for 20-β-hydroxyecdysone and cordifolioside A was performed at 254 nm and for columbin at 600 nm after derivatization with anisaldehyde‒sulfuric acid. The optimized mobile phase resulted in chromatographic separation of peaks for cordifolioside A, 20-β-hydroxyecdysone, and columbin at RF of 0.12, 0.47, and 0.86, respectively. The linear concentration range was found to be 750‒2250 ng/band for 20-β-hydroxyecdysone and cordifolioside A and 675‒1875 ng/band for columbin with (r2 > 0.99). The methodology showed good recoveries as 98.96‒101.43% for cordifolioside A, 98.15‒101.56% for 20-β-hydroxyecdysone, and 98.06‒98.80% for columbin. The limit of detection was found for columbin, 20-β-hydroxyecdysone, and cordifolioside A as 53.86 ng/band, 40.90 ng/band, and 107.05 ng/band, while the limit of quantification was found to be 163.21 ng/band, 123.94 ng/band, and 324.38 ng/band, respectively. The relative standard deviation for precision and robustness study for all the markers was found to be within 2%. Three markers were identified and confirmed in T. cordifolia stem extracts by ESI‒MS/MS. Compounds were assigned as norditerpene furan glycosides, ecdysteroids, and diterpenoid furanolactone: cordifolioside A (m/z = 527 [M + Na]+; UV λmax 221 nm), 20-β-hydroxyecdysone (m/z = 481.30 [M + H]+; UV λmax 247 nm), and columbin (m/z = 359 [M + H]+; UV λmax 210 nm). The optimized method was found accurate, reproducible, robust, and specific and can be applied for the quantification of cordifolioside A, 20-β-hydroxyecdysone, and columbin for quality control of extracts of T. cordifolia. Supplementary Information The online version contains supplementary material available at 10.1007/s00764-021-00115-7.

Dataset Information

Identification and quantification of cannabinol as a biomarker for local hemp retting in an ancient sedimentary record by HPTLC-ESI-MS.

Publications

Identification and quantification of cannabinol as a biomarker for local hemp retting in an ancient sedimentary record by HPTLC-ESI-MS.

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