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High-Resolution Mass Spectrometry (HRMS)01:15

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The resolution of a mass spectrometer depends on the efficiency of separating ions with different ion masses. The mass of an atom is approximated to the sum of the masses of protons and neutrons inside, considering the masses of protons and neutrons as equal. However, the masses of the proton (1.6726 × 10−24 g) and neutron (1.6749 × 10−24 g) are not truly equal. There is a minor error in the expression of atomic masses relative to the simplest atom of hydrogen. For...
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Optimized Extraction Method for Neutral Cannabinoids Quantification Using UHPLC-HRMS/MS.

João Victor Meirelles1,2, Débora Cristina Diniz Estevam2, Vanessa Farelo Dos Santos2

  • 1Departamento de Química, Pontifícia Universidade Católica do Rio de Janeiro, Rio de Janeiro 22451-045, RJ, Brazil.

Biomolecules
|February 26, 2025
PubMed
Summary
This summary is machine-generated.

Optimized extraction methods for cannabis herbal extracts (CHE) improve the analysis of key cannabinoids like CBD, THC, and CBN. This faster, cheaper, and reliable approach ensures accurate pharmaceutical quality control for human and veterinary medicines.

Keywords:
Box–Behnken designCannabis herbal extractsFull Factorial DesignUHPLC-HRMS/MScannabinoids

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Area of Science:

  • Analytical Chemistry
  • Pharmacognosy
  • Forensic Science

Background:

  • The global cannabis market is growing, increasing demand for cannabis herbal extracts (CHE) in clinical applications.
  • Neutral cannabinoids like cannabidiol (CBD), tetrahydrocannabinol (THC), and cannabinol (CBN) are key active compounds in CHE.
  • Non-standardized cannabinoid content in CHE presents challenges for pharmaceutical quality control and therapeutic efficacy.

Purpose of the Study:

  • To develop and optimize a multivariate method for extracting CBD, THC, and CBN from commercial CHE.
  • To validate a predictive model using Response Surface Methodology for extraction efficiency.
  • To establish a rapid, cost-effective, and reliable analytical method for cannabinoid quantification in CHE.

Main Methods:

  • Utilized Full Factorial and Box-Behnken designs for optimizing extraction parameters.
  • Employed methanol/hexane (9:1 v/v) solvent system with minimal volume and short extraction times.
  • Quantified cannabinoids using ultra-high-performance liquid chromatography coupled to high-resolution tandem mass spectrometry (UHPLC-HRMS/MS).

Main Results:

  • Agitation and sonication times were identified as critical extraction parameters, followed by solvent volume.
  • The optimized method demonstrated high precision (<15%), accuracy (69-98%), sensitivity (23-39 ng kg-1), and linearity.
  • Successfully processed 16 commercial CHE samples within a 3-hour timeframe, proving practicality and reproducibility.

Conclusions:

  • Developed a significantly faster, cheaper, and more efficient protocol for cannabinoid extraction compared to existing literature methods.
  • Achieved state-of-the-art analytical sensitivity and specificity using UHPLC-HRMS/MS for reliable routine analysis.
  • The validated method is suitable for quality control of commercial CHE in both human and veterinary pharmaceutical applications.