Advanced Cannabinoid Analysis - Latest Method Developments

Separating Cannabinoid Stereoisomers Utilizing LabSolutions MD with an Analytical Quality by Design (AQbD) Approach

Separating Cannabinoid Stereoisomers Utilizing LabSolutions MD with an Analytical Quality by Design (AQbD) Approach

The cannabis market has been rapidly growing with the list of identified cannabinoids constantly increasing. Analytical methods for detecting over 25 cannabinoids by means of HPLC (High Pressure Liquid Chromatography) analysis have been explored and currently there are methods to separate 21 cannabinoids in a single run. Expanding the list of cannabinoids is possible, however stereoisomers challenge the current methods and, therefore, further method optimization is needed. Shimadzu’s new analytical method development software, LabSolutions MD (Method Development) alleviates the tedious task of testing, analyzing, and comparing all the individual runs. LabSolutions MD uses “Analytical Quality by Design (AQbD)” concepts to determine the optimal method for cannabinoid separation. Experimental design during the entire method development process, identification of the most robust analytical conditions, and predicted of chromatograms, provide the user with the power to automate the development of robust analytical methods. This software can be an asset to many fields and will be used in this study to efficiently separate cannabis stereoisomers.

The Quantitation and Simultaneous InSource Fragmentation of 16 Cannabinoids in Hemp Using Single Quadrupole LC-MS

The Quantitation and Simultaneous In-Source Fragmentation of 16 Cannabinoids in Hemp Using Single Quadrupole LC-MS

With the passing of the Farm Bill in December 2018, which legalized hemp if the psychoactive compound, THC, content is 0.3% or less, and the legalization of cannabis in more than two thirds of US states and Canada, more accurate and sensitive analytical methods are needed for the quantitative determination of cannabinoids besides the widely applied technique of HPLC with UV and photodiode array detectors. The higher sensitivity, specificity, and mass identification provided by LC-MS are increasingly recognized for the quantitative determination of cannabinoids. In a previous application note (HPLC-028), an in-source fragmentation (SID) method was developed using the Shimadzu single quadrupole MS (LCMS-2020) to characterize 16 cannabinoids.

In this extended study, an LC-MS method of quantitation and simultaneous SID was developed using the LCMS-2020 single quadrupole MS with an integrated LC front end (LC 2040C 3D) for the quantification of 16 cannabinoids, including ∆9- tetrahydrocannabinol (∆9-THC), ∆8- tetrahydrocannabinol (∆8-THC), cannabidiol (CBD), cannabigerol (CBG), cannabinol (CBN), cannabicyclol (CBL) and their respective acidic forms, etc. Selected ion monitoring (SIM) was used for quantitation, simultaneous positive and negative scans were used for identification.

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