scholarly journals A Quantitative 1H-NMR Method for Screening Cannabinoids in CBD Oils

Author(s):  
Ines Barthlott ◽  
Andreas Scharinger ◽  
Patricia Golombek ◽  
Thomas Kuballa ◽  
Dirk W. Lachenmeier

Toxicologically relevant levels of the psychoactive ∆9-tetrahydocannabinol (∆9-THC) as well as high levels of non-psychoactive cannabinoids potentially occur in CBD (cannabidiol) oils. For consumer protection in the fast-growing CBD oil market, facile and rapid quantitative methods to determine the cannabinoid content are crucial. However, the current standard method, i.e., liquid chromatography combined with tandem mass spectrometry (HPLC-MS/MS), requires a time-consuming multistep sample preparation. In this study, a quantitative nuclear magnetic resonance spectroscopy (qNMR) method for screening cannabinoids in CBD oils was developed. Contrary to the HPLC-MS/MS method, this qNMR features a facile sample preparation, i.e., only diluting the CBD oil in deuterochloroform. Pulse length-based concentration determination (PULCON) enables a direct quantification using an external standard. The signal intensities of the cannabinoids were enhanced during the NMR spectra acquisition by means of multiple suppression of the triglycerides which are a major component of the CBD oil matrix. The validation confirmed linearity for CBD, cannabinol (CBN), ∆9-THC and ∆8-THC in hemp seed oil with sufficient recoveries and precision for screening. Comparing the qNMR results to HPLC-MS/MS data for 46 commercial CBD oils verified the qNMR accuracy for ∆9-THC and CBD but with higher limits of detection. The developed qNMR method paves the way for increasing the sample throughput as a complementary screening before HPLC-MS/MS.

Toxics ◽  
2021 ◽  
Vol 9 (6) ◽  
pp. 136
Author(s):  
Ines Barthlott ◽  
Andreas Scharinger ◽  
Patricia Golombek ◽  
Thomas Kuballa ◽  
Dirk W. Lachenmeier

Toxicologically relevant levels of the psychoactive ∆9-tetrahydocannabinol (∆9-THC) as well as high levels of non-psychoactive cannabinoids potentially occur in CBD (cannabidiol) oils. For consumer protection in the fast-growing CBD oil market, facile and rapid quantitative methods to determine the cannabinoid content are crucial. However, the current standard method, i.e., liquid chromatography combined with tandem mass spectrometry (HPLC-MS/MS), requires a time-consuming multistep sample preparation. In this study, a quantitative nuclear magnetic resonance spectroscopy (qNMR) method for screening cannabinoids in CBD oils was developed. Contrary to the HPLC-MS/MS method, this qNMR features a simple sample preparation, i.e., only diluting the CBD oil in deuterochloroform. Pulse length-based concentration determination (PULCON) enables a direct quantification using an external standard. The signal intensities of the cannabinoids were enhanced during the NMR spectra acquisition by means of multiple suppression of the triglycerides which are a major component of the CBD oil matrix. The validation confirmed linearity for CBD, cannabinol (CBN), ∆9-THC and ∆8-THC in hemp seed oil with sufficient recoveries and precision for screening. Comparing the qNMR results to HPLC-MS/MS data for 46 commercial CBD oils verified the qNMR accuracy for ∆9-THC and CBD, but with higher limits of detection. The developed qNMR method paves the way for increasing the sample throughput as a complementary screening before HPLC-MS/MS.


2020 ◽  
Vol 57 (6) ◽  
pp. 451-459
Author(s):  
Liujun Pei ◽  
Yuni Luo ◽  
Xiaomin Gu ◽  
Jiping Wang
Keyword(s):  
Seed Oil ◽  

2020 ◽  
Vol 57 (3) ◽  
pp. 230-236 ◽  
Author(s):  
Yawei Huang ◽  
Liujun Pei ◽  
Xiaomin Gu ◽  
Jiping Wang

Author(s):  
M.A. Asokan ◽  
S. Senthur Prabu ◽  
Anirudh Bollu ◽  
M. Abhinay Reddy ◽  
Aditya Ram ◽  
...  

2019 ◽  
Vol 15 (1) ◽  
Author(s):  
Vibha Devi ◽  
Shabina Khanam

Abstract In the present work, supercritical fluid extraction (SFE) of hemp (Cannabis sativa) seed oil at various ranges of SFE parameters is performed. These parameters and respective ranges are temperature (40–80) °C, pressure (200–350) bar, solvent (CO2) flow rate (5–15) g/min, particle size (0.43–1.02) mm and amount of co-solvent (ethanol) (0–10) % of solvent flow rate. Central composite design (CCD) suggests 32 experimental runs to perform through SFE. The obtained oil is analysed through gas chromatography to identify its fatty acids concentrations. The ratio of ω-6 linoleic and ω-3 α-linolenic fatty acids (ω-6/ω-3) is optimized through CCD to obtain the desired amount of 3:1 as this ratio is highly preferred for various health benefits. Ratio of ω-6/ω-3 is obtained in the range from 2.11 to 3.06:1 for all experimental runs. The effect of SFE parameters on this ratio is investigated. Further, cross-validation is peformed on the experimental data obtained for the concentrations of both fatty acids by jackknife and bootstrap resampling to authenticate the obtained data. Small value of standard deviation (~1), less standard error of the mean (SEM) (<0.8) and less variance coefficient (<0.11) confirms the validity of the obtained data. All the estimators’ values such as standard deviation, variance coefficients and SEM are observed in 95 % of confidence intervals.


Molecules ◽  
2018 ◽  
Vol 23 (5) ◽  
pp. 1131 ◽  
Author(s):  
Katarzyna Tyśkiewicz ◽  
Roman Gieysztor ◽  
Izabela Maziarczyk ◽  
Paweł Hodurek ◽  
Edward Rój ◽  
...  

Poljoprivreda ◽  
2019 ◽  
Vol 25 (1) ◽  
pp. 81-88 ◽  
Author(s):  
Mario Jakobović ◽  
Stela Jokić ◽  
Melita Lončarić ◽  
Snježana Jakobović ◽  
Krunoslav Aladić ◽  
...  

Aim of this study was to monitor the influence of drying method (naturally and chamber drying) and different sample preparation on supercritical CO2 extraction of oil from three grape seed varieties (Graševina, Zweigelt, Cabernet Sauvignon). The highest oil content was obtained from naturally dried screened and washed seeds of red variety Cabernet Sauvignon (14.85%) and lowest from chamber dried screened seeds of white variety Graševina (7.67%). Peroxide value ranged from 0.36 to 1.77 mmol O2/kg oil, free fatty acids 0.28-8.0%, and insoluble impurities 0.05-0.28%. Determined fatty acids were palmitic (6.98-11.58%), stearic (3.82-6.59%), oleic (14.90-19.97%) and linoleic acid (61.82-71.96%) in oil obtained from naturally dried seeds and 6.84-8.68%, 4.12-5.73%, 15.10-20.18% and 67.88-70.76% in oil from chamber dried seeds, respectively. In defatted cakes after supercritical CO2 extraction, protein and fibre content ranged from 8.17 to 9.85% and 34.58 to 43.96%, respectively. According to ANOVA results, sample preparation and drying method had statistically significant influence on grape seed oil extraction.


2009 ◽  
Vol 72 (8) ◽  
pp. 1774-1789 ◽  
Author(s):  
BYRON BREHM-STECHER ◽  
CHARLES YOUNG ◽  
LEE-ANN JAYKUS ◽  
MARY LOU TORTORELLO

Advances in molecular technologies and automated instrumentation have provided many opportunities for improved detection and identification of microorganisms; however, the upstream sample preparation steps needed to apply these advances to foods have not been adequately researched or developed. Thus, the extent to which these advances have improved food microbiology has been limited. The purpose of this review is to present the current state of sample preparation, to identify knowledge gaps and opportunities for improvement, and to recognize the need to support greater research and development efforts on preparative methods in food microbiology. The discussion focuses on the need to push technological developments toward methods that do not rely on enrichment culture. Among the four functional components of microbiological analysis (i.e., sampling, separation, concentration, detection), the separation and concentration components need to be researched more extensively to achieve rapid, direct, and quantitative methods. The usefulness of borrowing concepts of separation and concentration from other disciplines and the need to regard the microorganism as a physicochemical analyte that may be directly extracted from the food matrix are discussed. The development of next-generation systems that holistically integrate sample preparation with rapid, automated detection will require interdisciplinary collaboration and substantially increased funding.


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