HRMS Detector for the New HILIC CBD Method Development in Hemp Seed Oil

Wang, Yu; Hao, Zhigang; Pan, Long

doi:10.1021/jasms.0c00331

Cited by 5 publications

(6 citation statements)

References 42 publications

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“…The challenge to simultaneously quantify CBD and hemp seed oil TAG was reported in our previous study [11]. We found that the common mobile phases like methanol and acetonitrile cannot effectively elute TAGs out from reverse phase columns.…”

Section: Introductionmentioning

confidence: 76%

“…The next challenge was how to characterize the separated TAG peak as a chemical marker for CBD hemp seed oil quantification. The TAG structures can be profiled and characterized by using chromatographic techniques [11,21]. Fragmentation patterns and neutral loss in mass spectrometry have been used for the quantification of regioisomers with minimal standards [22,23], and the online acetone Paterno-Buchi reaction and ultraviolet photo-dissociation coupled with mass spectrometry was recently used to determine the double bond position in TAG structures [24,25].…”

Section: Introductionmentioning

confidence: 99%

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HPLC Method for Separation of Cannabidiol Hemp Seed Oil with Skin Lipids and Tandem HRMS Technology for Characterization of a Chemical Marker

et al. 2021

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Cannabidiol (CBD) hemp seed oil is a commercial raw material with antioxidant and anti-inflammatory benefits that has been formulated into body wash and skin care products. The biggest analytical challenge is how to simultaneously quantify CBD and hemp seed oil as they deposited on the skin surface. CBD is easily separated and quantified from skin surface extracts via a HPLC-mass spectrometry methodology. However, the structural skeleton of triacylglycerides (TAGs) in hemp seed oil is same as those from the skin surface sebum. The strong hydrophobicity with subtle structural difference challenges their separation. In this project, a new reverse phase HPLC-high resolution mass spectrometry methodology was developed with a strong mobile phase normal propanol. The separated hemp seed oil TAGs in the chromatogram were identified and characterized using data-dependent acquisition (DDA) technology. Based on the daughter ion characterization, the separated peak with an ammonium adduct at 890.7226 [M + NH4]+ was confirmed as the parent ion of glycerol with three omega-3 fatty acid chains. This is the first time TAG structure with direct HPLC-tandem mass spectrometry technology has been elucidated without a hydrolysis reaction. The confirmed TAG structure with an ammonium adduct at 890.7226 ± 0.0020 can be used as a representative chemical marker for the hemp seed oil quantification.

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Section: Introductionmentioning

confidence: 76%

Section: Introductionmentioning

confidence: 99%

HPLC Method for Separation of Cannabidiol Hemp Seed Oil with Skin Lipids and Tandem HRMS Technology for Characterization of a Chemical Marker

et al. 2021

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“…The RSDs of the CBD calibrators used to develop the calibration curves were less than 10%, and no analyte signal was observed in the unspiked chocolate and gummy matrices (example shown in Figure S6). Several studies (presented in Table ) have reported the successful quantification of cannabinoids in Cannabis -infused matrices such as oils/liquids, ,,,− ,,− food products, ,,,,,,− concentrates, capsules, ,, and vape products. , Ciolino et al reported the average percent (%) recovery of five cannabinoids in various spiked matrices, including edible oils, foods, topicals, oral OTC (over-the-counter) pharmaceuticals, beverages, and dairy foods . Included within the food product category were milk and dark chocolate bars (extracted with acetonitrile) and a hard candy (extracted with 83% aqueous acetonitrile) …”

Section: Resultsmentioning

confidence: 99%

DART-MS Facilitated Quantification of Cannabinoids in Complex Edible Matrices─Focus on Chocolates and Gelatin-Based Fruit Candies

2023

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Traditional methods for detecting and quantifying cannabinoids in Cannabis sativa materials are most often chromatography-based, and they generally require extensive sample preparation protocols to render materials into a form that can be injected into the systems without the risk of contaminating or damaging the equipment. This challenge is amplified when interrogating the increasingly broad range of matrix types that cannabinoids are infused within, such as edibles that also contain sugars, fats, lipids, and carbohydrates. The requisite application of highly nuanced methods that must be developed for each matrix type is, in addition to being resource-intensive and time-consuming, highly impractical and unsustainable for crime laboratories endeavoring to perform such analyses in a routine manner, since they are often under-resourced while typically also confronting sample testing backlogs. A key to resolving this issue is to identify an analysis approach that avoids the requirement for nuanced method development by being applicable to a broader range of matrix types. Ambient ionization mass spectrometry (AIMS) methods have shown great promise in their ability to rapidly interrogate samples. Therefore, this study focused on developing validated protocols using AIMS (specifically, direct analysis in real time-high-resolution mass spectrometry, or DART-HRMS) to detect and quantify Δ9-tetrahydrocannabinol (THC) and cannabidiol (CBD) in edible matrices. Calibration curves were developed using deuterated counterparts of THC and CBD as internal standards. Following the use of high cannabinoid recovery rate extraction protocols for chocolates and gelatin-based fruit candies or “gummies”, the DART-HRMS approach was applied to quantify cannabinoid levels in commercially available cannabinoid-infused candies, yielding results similar to those reported on the product labels. Importantly, the developed method circumvented challenges encountered using traditional approaches. As the Cannabis field continues to evolve and new matrix types emerge on the market, the DART-HRMS detection and quantification protocols can be readily applied without the need for major procedural adaptations.

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“…In addition, the core silica material used in normal phase HPLC provides alternative retaining power by adsorptive interaction, which was thoroughly described by Prof. Irgum in his HILIC methodology review [42]. This adsorptive interaction between core silica and analytes can be easily observed in cannabidiol (CBD) separation from hemp seed oil by the HILIC method when the ACN concentration reaches 99% [43]. This interaction provides additional separation opportunities for complicated analytes, especially when several types of functional groups were present [44].…”

Section: Resultsmentioning

confidence: 99%

Evaluation of multiple hydrophilic interaction chromatography columns and surrogate matrix for arginine quantification in saliva by high‐resolution mass spectrometry

Wang

Hao

Pan

2021

J of Separation Science

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Arginine, a pivotal ingredient in many biochemical synthetic pathways, can be used as a biomarker for many oral care clinical applications. It is still a challenge to develop a sensitive and reliable chromatographic method to quantify arginine as a biomarker in saliva, with or without arginine product pretreatment. The current method solved two critical issues for arginine quantitation in human saliva.The first issue was how to optimize arginine peak shape. A hydrophilic interaction chromatography method based on the column selection, pH and pK a relationship, mobile phase ionic strength, organic solvent consideration, and temperature effects was developed. An optimized chromatographic condition for arginine quantitation in the saliva matrix was obtained. The second issue was how to build confidence in the use of a simple surrogate matrix methodology to replace the more complex traditional standard addition methodology. The surrogate matrix methodology we developed is applicable to the measurement of arginine as a potential non-invasive biomarker in human saliva. The method detection and quantification limit reached 2 and 6 ng/mL. The tailing factor was within the 0.9-1.1 range even though arginine had three pK a values at 2.18, 9.09, and 13.2. K E Y W O R D Sarginine, hydrophilic interaction chromatography, retention mechanism, saliva, surrogate matrix method INTRODUCTIONArginine (2-amino-5-guanidinovaleric acid) has been studied for over 100 years since it was first isolated from lupin seedlings in 1886 [1]. Based on current understanding, arginine is considered a semi or conditionally essential amino acid to human beings. The term semi-essential is Article Related Abbreviations: HRMS, high-resolution mass spectrometry; SAM, standard addition method; SLS, sodium lauryl sulfate; SMM, surrogate matrix method commonly applied to amino acids that are produced from other essential amino acids and these amino acids may be acquired from the diet if there is not a sufficient amount of precursors or if the biosynthetic system is defective. Arginine occupies a central position in multiple biosynthetic pathways including protein synthesis, the urea/ornithine cycle, polyamine synthesis, and nitric oxide production [1,2]. Arginine has been involved in diverse cellular processes ranging from redox balance to cell cycles, and processes for clinical applications [3], such as in the prevention and treatment of cardiovascular diseases, Type II diabetes, 3580

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HRMS Detector for the New HILIC CBD Method Development in Hemp Seed Oil

Cited by 5 publications

References 42 publications

HPLC Method for Separation of Cannabidiol Hemp Seed Oil with Skin Lipids and Tandem HRMS Technology for Characterization of a Chemical Marker

HPLC Method for Separation of Cannabidiol Hemp Seed Oil with Skin Lipids and Tandem HRMS Technology for Characterization of a Chemical Marker

DART-MS Facilitated Quantification of Cannabinoids in Complex Edible Matrices─Focus on Chocolates and Gelatin-Based Fruit Candies

Evaluation of multiple hydrophilic interaction chromatography columns and surrogate matrix for arginine quantification in saliva by high‐resolution mass spectrometry

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