Cannabinoid Content and Label Accuracy of Various Hemp-Derived Haircare, Cosmetic, and Edible Products Available at Retail Stores and Online in the United States.

Aim: To evaluate the label accuracy and content of various hemp-derived cannabidiol (CBD) products (cannabinoid products with ≤0.3% Δ9-tetrahydrocannabinol [THC]), as well as evaluate advertised claims on product labels. Methods: Hemp haircare, cosmetics, and food/drink products that were advertised to contain CBD were purchased from retail stores in the Baltimore, Maryland area (purchased in July 2020) and online (purchased in August 2020). Cannabinoid concentrations were measured using gas chromatography-mass spectrometry. Percent deviations between labeled and actual CBD concentrations were determined. Label information such as references to the Food and Drug Administration (FDA), external testing claims, and other claims (i.e., cosmetic or beauty, therapeutic, health halo effect, or "other") were quantified. Results: Ninety-seven products were purchased (35 in-store, 62 online). Of the 71 products with a specific total CBD amount on the label, 35 (49%) were underlabeled (>10% more CBD than advertised), 27 (38%) were overlabeled (>10% less CBD than advertised), and 9 (12.7%) were accurately labeled (within ±10% of labeled CBD). The median (range) percentage deviations were -53% (-100%-76%) for haircare products, +18% (-100%-1076%) for cosmetics, and -1% (-100%-4468%) for food/drinks. CBD label accuracy did not differ significantly between products with external testing claims versus those without (t40 = 0.23, p = 0.82). Overall, 24% of the 97 (total) products made a cosmetic or beauty claim (e.g., "skin looks more youthful"), 40% made a therapeutic claim (e.g., "pain relief"), and 86% made a health halo effect claim (e.g., "paraben-free," "dye-free," etc.). Most products (63%) did not include a disclaimer that claims had not been evaluated by the FDA. Conclusions: Most of the products included in this sample were inaccurately labeled for CBD content, including those claiming to have been tested by third party laboratories. A notable finding was that 10 products did not contain any CBD. Many products made therapeutic claims or used marketing tactics to seemingly convey they were safe/healthy, but only about one-third included disclaimers that these statements had not been evaluated by the FDA. These findings highlight the need for proper regulatory oversight of cannabinoid-containing products to ensure quality assurance and deter misleading or unfounded health claims in product marketing.

Stability of Nano-Emulsified Cannabidiol in Acidic Foods and Beverages.

Introduction: Food and beverage products containing cannabidiol (CBD) is a growing industry, but some CBD products contain Δ9-tetrahydrocannabinol (Δ9-THC), despite being labeled as "THC-free". As CBD can convert to Δ9-THC under acidic conditions, a potential cause is the formation of Δ9-THC during storage of acidic CBD products. In this study, we investigated if acidic products (pH ≤ 4) fortified with CBD would facilitate conversion to THC over a 2-15-month time period. Materials and Methods: Six products, three beverages (lemonade, cola, and sports drink) and three condiments (ketchup, mustard, and hot sauce), were purchased from a local grocery store and fortified with a nano-emulsified CBD isolate (verified as THC-free by testing). The concentrations of CBD and Δ9-THC were measured by Gas Chromatography Flame Ionization Detector (GC-FID) and Liquid Chromatography with tandem mass spectrometry (LC-MS/MS), respectively, for up to 15 months at room temperature. Results: Coefficients of variation (CVs) of initial CBD concentrations by GC-FID were <10% for all products except ketchup (18%), showing homogeneity in the fortification. Formation of THC was variable, with the largest amount observed after 15 months in fortified lemonade #2 (3.09 mg Δ9-THC/serving) and sports drink #2 (1.18 mg Δ9-THC/serving). Both beverages contain citric acid, while cola containing phosphoric acid produced 0.10 mg Δ9-THC/serving after 4 months. The importance of the acid type was verified using acid solutions in water. No more than 0.01 mg Δ9-THC/serving was observed with the condiments after 4 months. Discussion: Conversion of CBD to THC can occur in some acidic food products when those products are stored at room temperature. Therefore, despite purchasing beverages manufactured with a THC-free nano-emulsified form of CBD, consumers might be at some risk of unknowingly ingesting small amounts of THC. The results indicate that up to 3 mg Δ9-THC from conversion can be present in a serving of CBD-lemonade. Based on the previous studies, 3 mg Δ9-THC might produce a positive urine sample (≥15 ng/mL THC carboxylic acid) in some individuals. Conclusion: Consumers must exert caution when consuming products with an acidic pH (≤4) that suggests that they are "THC-Free," because consumption might lead to positive drug tests or, in the case of multiple doses, intoxication.

LC-MS-MS Analysis of N,α-Diethylphenethylamine (N,α-ETH) and Its Positional Isomer N,ß-Diethylphenethylamine (N,ß-ETH) in Dietary Supplements.

In a previous publication, we reported on the analysis of several dietary supplement/exercise formulas and the quantitation of N,α-diethylphenethylamine (N,α-ETH, 3: ). In this article we report on the reanalysis of these products using LC-MS-MS and GC-MS methods capable of clearly separating the N,α-isomer ( 3: ) from its N,ß-isomer (N,ß-ETH, 4: ). The reanalysis, by both methods, showed that all samples previously reported as containing N,α-ETH ( 3: ) do contain only that isomer with no detectable concentrations of the N,ß-ETH ( 4: ).

Methylhexanamine is not detectable in Pelargonium or Geranium species and their essential oils: A multi-centre investigation.

In an earlier study, we developed two sensitive and reliable procedures for gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis of methylhexaneamine (MHA) in P. graveolens plant materials and volatile oils. None of the analyzed plant materials or oils showed any detectable levels of MHA which was further substantiated by high resolution liquid chromatography-quantum time of flight-mass spectrometry (LC-QTOF-MS) analysis with a limit of detection of 10 ppb. However, other laboratories (two studies) reported the presence of MHA in some samples of P. graveolens and pelargonium oil acquired by the investigators from China. Because of the controversy of whether Pelargonium species or pelargonium oil contains MHA, it was recommended that splits of multiple samples be analyzed by different laboratories. In this investigation, multiple plant materials and oil samples were collected from around the world. These samples were submitted to four different sites for analysis. All sites adopted a similar extraction method. All the analysis sites used LC-MS/MS or LC-QTOF-MS and detection limit was set close to the 10 ng/mL as previously reported. A total of 18 plant samples belonging to 6 different Pelargonium species and 9 oils from different locations around the world were split among 4 different analytical laboratories for analysis (each lab received the same samples). None of the laboratories detected MHA in any of the samples at or around the 10 ppb detection level of the procedure used.

Pelargonium oil and methyl hexaneamine (MHA): analytical approaches supporting the absence of MHA in authenticated Pelargonium graveolens plant material and oil.

Methylhexaneamine (MHA) has been marketed in dietary supplements based on arguments that it is a constituent of geranium (Pelargonium graveolens) leaves, stems, roots or oil, and therefore qualifies as a dietary ingredient. The purpose of this study is to determine whether P. graveolens plant material (authenticated) or its oil contains detectable quantities of MHA. Two analytical methods were developed for the analysis of MHA in P. graveolens using gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry. The results were further confirmed using liquid chromatography-high-resolution mass spectrometry. Twenty commercial volatile oils, three authenticated volatile oils and authenticated P. graveolens leaves and stems (young and mature, and fresh and dried) were analyzed for MHA content. In addition, three dietary supplements containing MHA that alleged P. graveolens as the source are analyzed for their MHA content. The data show that none of the authenticated P. graveolens essential oils or plant material, nor any commercial volatile oil of Pelargonium (geranium oil) contain MHA at detectable levels (limit of detection: 10 ppb). The dietary supplements that contained MHA as one of their ingredients (allegedly from geranium or geranium stems) contained large amounts of MHA. The amounts of MHA measured are incompatible with the use of reasonable amounts of P. graveolens extract or concentrate, suggesting that MHA was of synthetic origin.

Liquid chromatography-tandem mass spectrometry analysis of urine specimens for K2 (JWH-018) metabolites.

Marijuana is the most widely used drug of abuse all over the world. The major active constituent of the drug is Δ9- tetrahydrocannabinol (Δ9-THC). Δ9-THC exerts its psychological activities by interacting with the cannabinoid receptors (CB1 and CB2) in the brain. JWH-018, HU-210, and CP-47497, with CB1 agonist activity (similar to Δ9-THC), have been used by the drug culture to spike smokable herbal products to attain psychological effects similar to those obtained by smoking marijuana. The products spiked with these CB1 agonists are commonly referred to as "Spice" or "K2". The most common compound used in these products is JWH-018 and related compounds (JWH-073 and JWH-250). Little work has been done on the detection of these synthetic cannabimimetic compounds in biological specimens. This report investigated the metabolism of JWH-018 by human liver microsomes, identification of the metabolites of JWH-018 in urine specimen of an individual who admitted use of the drug, and reports on the quantitation of three of its urinary metabolites, namely the 6-OH-, the N-alkyl OH (terminal hydroxyl)-, and the N-alkyl terminal carboxy metabolites using liquid chromatography-tandem mass spectrometry. The concentrations of these metabolites are determined in several forensic urine specimens.

LC-MS-(TOF) analysis method for benzodiazepines in urine samples from alleged drug-facilitated sexual assault victims.

In recent years there has been an increase in the number of reports in the U.S. of the use of drugs to commit sexual assault. In 1994, a nationwide urine testing program was developed to assess the incidence of the use of drugs to facilitate sexual assault and provide information for use in the investigation of these crimes. Urine samples were collected from victims of suspected drug-induced sexual assault by law enforcement agencies, emergency rooms, and rape crisis centers. The most implicated drug class was benzodiazepines, either alone or in combination with alcohol. In this report, a procedure was developed for the screening of 22 benzodiazepines in human urine by liquid chromatography-time of flight-mass spectrometry [LC-MS-(TOF)]. The limit of quantitation for all benzodiazepines ranged from 2 to 10 ng/mL, and the limit of detection was 0.5 to 3.0 ng/mL. These results suggest that the method sensitivity is suitable to screen for all 22 benzodiazepines in human urine at low levels. The method was used to analyze samples previously reported to have screened positive for benzodiazepines by immunoassay at 50 ng/mL cut off but failed to confirm by a gas chromatography-MS method. The results of reanalysis of these samples using this LC-MS method are reported.