Determination of cannabinoids in hemp nut products in Taiwan by HPLC‐MS/MS coupled with chemometric analysis: quality evaluation and a pilot human study

Abstract

Hemp nuts are mature cannabis seeds obtained after shelling and that are commonly used in traditional Chinese medicine for treating functional constipation. In this work, we screened hemp nut products, classified them, and verified the legality of consuming them. A total of 18 products were purchased from Taiwan, China, and Canada. Validated high-performance liquid chromatography with tandem mass spectrometry methods were developed for analyzing the cannabinoid (i.e., Δ -tetrahydrocannabinol (THC), cannabidiol (CBD), and cannabinol) content of the products and the concentration of urinary 11-nor-9-carboxy-THC. Chemometric techniques, namely hierarchical clustering analysis (HCA) and principal component analysis (PCA), were applied for rapidly classifying 11 concentrated powder products in Taiwan. A pilot human study comprising single and multiple administrations of a product with 1.5 µg/g of THC was conducted to examine the urinary 11-nor-9-carboxy-THC concentration. Through optimization of 3 full factorial design, using 60% isopropanol as the extraction solvent exhibited the highest yield of cannabinoids and was applied as the optimal condition in further analysis. The results of HCA and PCA on quality evaluation were in good agreement; however, the tested products possessed distinct CBD-to-THC ratios which ranged widely from 0.1:1 to 46.8:1. Particularly, the products with CBD-to-THC ratios higher than 1:1 were the majority in Taiwan. Our data suggested that all the tested hemp nut products met the Taiwan restriction criterion of 10 µg/g of THC. We propose a usual consumption amount of hemp nut products in Taiwan would unlikely to violate the cut-off point of 15 ng/mL of urinary 11-nor-9-carboxy-THC. Copyright © 2016 John Wiley & Sons, Ltd.

A review on the recent advances in HPLC, UHPLC and UPLC analyses of naturally occurring cannabinoids (2010–2019)

“…Various HPLC and UPLC methods that have been reported for the analysis of cannabinoids in C. sativa L. plant samples and Cannabis consumer products, e.g. hashish, marijuana and cannabis oils, since the year 2010, are summarised in Tables and , and appraised in the following subsections.…”

“…Various LC‐based analytical techniques have become quite popular in the analysis of cannabinoids in Cannabis consumer products, which include smoking products, e.g. hashish and marijuana, cannabidiol oil, Cannabis olive oil, Cannabis tinctures, Cannabis medicinal products and Cannabis tea (Table ) . In the HPLC and UPLC (or UHPLC) methods, the use of PDA or MS detection technologies have become routine for the analysis of Cannabis consumer products.…”

“…There have been at least 11 different HPLC methods published during the last decade for the analysis of commercial Cannabis using either a HPLC‐UV‐PDA or HPLC‐MS/MS techniques . Cannabidiol (CBD, 3 )‐based oil preparations have become one of the most popular consumer products because of a variety of beneficial effects of CBD ( 3 ), which is not a controlled substance, on human health .…”

Ephedra alkaloid contents of Chinese herbal formulae sold in Taiwan

“…Calibration curves were validated within the ranges 3–24 μg/mL for NE, NPE, and ME; 24–192 μg/mL for E; and 12–96 μg/mL for PE. Intra‐ and inter‐day variations were analyzed using the method of Chang et al to evaluate the accuracy and precision of the analytical method. Accuracy ranged from 102.5% to 105.0%, whereas precision – as indicated by the relative standard deviation – ranged from 1.1% to 4.1% (Table ).…”

Potential Risk of Higenamine Misuse in Sports: Evaluation of Lotus Plumule Extract Products and a Human Study

“…The subsequent processes before HPLC analysis were the same as those in the methods described in the preceding sections. All commercial products were subjected to HCA and PCA using R language version 3.1.2 as described previously [17]. Cluster analysis is a multivariate technique that arranges components on the basis of their characteristics.…”