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You are here: Home / NMR / Hemp – the role of cannabinoid analysis in farming, processing, product development, and product monitoring – 1H qNMR and HPLC method development

Hemp – the role of cannabinoid analysis in farming, processing, product development, and product monitoring – 1H qNMR and HPLC method development

January 30, 2020 by process nmr NMR

Callan McLoughlin of Process NMR Associates will be presenting analytical work we have performed on hemp raw materials and products. Below is the information on the talk.

The Mid-Hudson Section of the American Chemical Society Presents:

Hemp – the role of cannabinoid analysis in farming, processing, product development, and product monitoring – 1H qNMR and HPLC method development

Callan McLoughlin, Process NMR Associates, LLC and Ron Spadafora, Spadafarm, LLC

Date: February 27th, 2020, at 7pm – Light Refreshments will be served from 6:30 pm

Place: Vassar College, Bridge for Laboratory Sciences, Room 217

With the recent legalization of Hemp Cannabis sativa nationwide, and the rapidly expanding market for cannabidiol (CBD) products, there has been an increasing demand for phytochemical and cannabinoid analysis. A brief description will be provided on the Industrial Hemp Research Initiative in New York State. In recent years, the accepted gold standard for cannabinoid detection and quantification has been High Performance Liquid Chromatography (HPLC). Although this method has been successful, HPLC requires a large volume of solvents and regular calibration with expensive standards of the cannabinoids of interest. In conjunction with in-house HPLC method development, an independent quantitative Nuclear Magnetic Resonance (qNMR) spectroscopy approach was developed for the detection and quantification of cannabinoids such as THC, THCA, CBD, CBDA and CBN. Rapid extraction procedures utilizing deuterated chloroform for immediate qNMR hemp analysis were developed and standardized. The qNMR method developed was subsequently validated by HPLC, confirming the methods efficacy. Furthermore, the HPLC and qNMR methods are being validated in a University of Kentucky proficiency testing program comprising the statistical analysis of results on round-robin tests from 67 laboratories.

With access to a local hemp farm, an analysis of cannabinoid concentration based on flower location and plant maturation was performed. With a thorough understanding of the New York State hemp market, agriculture, and botanical processing, working with the farm was a useful partnership for the development of the analytical method and facilitation of the research. The height placement of flower and leaf location on the plant was found to significantly impact cannabinoid concentration. On average, hemp flower located near the top of the plant tested 15-20 wt% higher in potential CBD compared to hemp flower located near the bottom. Monitoring of hemp in the field was undertaken and a substantial increase (50-100 wt%) in cannabinoid concentration was observed during the final two weeks before harvest. Decarboxylation studies of CBDA to CBD was conducted at 105°C, 125°C, and 148°C over the course of an hour and the profiles of the rate of decarboxylation of CBDA to CBD were fit to a sigmoidal function. Finally, a number of topical and oral oil products, vape products, beverages, and edible gummy products were analyzed by 1H qNMR for CBD potency and quality assurance.

Bio: Callan McLoughlin is a graduate of Our Lady of Lourdes HS in Poughkeepsie and a 2019 graduate of Marist College obtaining a BA in Biochemistry. He currently works at Process NMR Associates in Poughkeepsie as an analytical chemist. He will be presenting this research at the National ACS meeting in Philadelphia on March 22. He is currently applying for Ph.D. programs in Chemistry for Fall 2020.

Bio: Ron Spadafora is CEO of Spadafarm in Lagrangeville, NY and is a New York State Industrial Hemp Research Partner licensed to grow, process and extract CBD hemp flower into CBD oil. He works closely with researchers from Cornell University and SUNY on hemp related research and is currently a Principal Investigator for phytoremediation projects that utilize hemp plants to remove heavy metals from wastewater and soil. He graduated from George Washington University in Washington, DC and spent most of his career working as a systems analyst helping stakeholders within organizations to streamline and automate business and scientific processes.

Note: This talk is open to the public and anyone interested in the topic is invited to attend.

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