Quality test of cannabidiol profiling in CBD oil products and evaluation of residual THC at high temperature based on liquid chromatography coupled with tandem mass spectrometry.

Cannabidiol (CBD) oil products are available in Japan as cosmetics, fragrances, food and items. Herein, quality testing of cannabinoid profiling in CBD oil products and the evaluation of possible residual tetrahydrocannabinol (THC) in these products using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was conducted. A simple, sensitive, and selective LC-MS/MS assay (electrospray positive ion mode) was employed for the simultaneous quantification of eight cannabinoids. This quantification with three different oil samples showed that accuracy rates ranged from 87.7 to 106.9% (RSD > 3.5%). Furthermore, the quantification limit of THC is 0.001 mg/g of CBD oil products for suitable levels lower than the regulatory value. Notably, this method was used to evaluate CBD oil products from the Japanese market. Additionally, we investigated the THC conversion in CBD oil products at a high temperature (70°C) which has a minor effect on CBD stability in oil products with additives. Herein, the developed LC-MS/MS assay is applied to monitor the quality of CBD, trace THC and other components in CBD oil products.

LC-MS/MS Assay for the Measurement of Cannabidiol Profiling in CBD Oil from Japanese Market and Application for Convertible Tetrahydrocannabinol in Acetic Acid Condition.

Cannabidiol (CBD), a major non-psychoactive cannabinoid, has a lot of attention due to its potential relaxing properties and led the trend in commercial CBD aroma/oral hemp seed oil from the Japanese market. In this study, a routine assay for evaluating CBD oil samples was performed using LC coupled with tandem mass spectrometry (LC-MS/MS) and was used to apply the convertible tetrahydrocannabinol (THC) in acetic acid conditions. Based on the electrospray positive ion mode, the detection of cannabidiolic acid (CBDA; m/z 359 > 219), cannabigerolic acid (CBGA; m/z 361 > 343), cannabigerol (CBG; m/z 317 > 193), CBD (m/z 315 > 193), THC (m/z 315 > 193) and cannabinol (CBN; m/z 311 > 223) was performed by satisfying separation with high density of C18 column. Oil samples (50 mg) were diluted with isopropanol (5 mL), to which stable isotope internal standards were added by dilution with methanol/water (50/50), and accuracy rates ranged from 97.8 to 102.2%. This method was used to evaluate the CBD oil products (5 kinds) from the Japanese market. Our survey found obvious counterfeit (non-detectable CBD) CBD oil from Japanese market. Following that, we investigated the conversion of THC in CBD oil samples in simple conditions such as 10% acetic acid and 70 °C for 6 h and discovered that converts THC proportions are approximately 5% ((THC content/CBD content) × 100) and <1.0%. Thus, our developed LC-MS/MS assay could be applied to monitor the CBD concentration and convertible THC from CBD oil.

Screening Method for the Quality Evaluation of Cannabidiols in Water-based Products Using Liquid Chromatography Tandem Mass Spectrometry.

A sensitive, useful and preliminary screening method was proposed to quantitate the containable cannabinoids most commonly included in mineral water and gummi candy products, specifically cannabidiol (CBD), cannabinol (CBN), 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCA), cannabigerol (CBG), and cannabidiolic acid (CBDA), using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) for quality evaluations. Based on the electrospray positive ion mode, the limit of detection and the limit of quantification values were 0.2 to 0.5 ng/mL and 0.8 and 2.0 ng/mL. Samples (0.5 g) were diluted by water/methanol (50/50), to which stable isotope internal standards were added; the recovery results appeared in range from 91.3 to 101.2%. This method was applied to evaluate CBD products (6 kinds) from the Japanese market. Our survey found obvious discrepancies between the labeling and the results were overserved in products. In addition, CBN, THCA, CBG, and CBDA were not detected in full-spectrum products that contained various cannabinoids that naturally occur in the cannabis plant. Thus, it is necessary to be able to verify the accurate concentration and impurity in various CBD products from the Japanese market as quickly as possible.