Determination of variability of terpenes and terpenoids in Cannabis sativa by gas chromatography-flame ionization detection and gas chromatography-mass spectrometry

Giovannoni, Sol; Lancioni, Carlina; Vaccarini, Cristian Adrián; Sedán, Daniela; Andrinolo, Darı́o; Castells, Cecilia Beatriz Marta

doi:10.1016/j.chroma.2022.463669

Cited by 9 publications

(8 citation statements)

References 19 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…100), an aliquot of 10 mL was taken for analysis. As outlined in the first paragraph, HS-SPME has been considered the analytical extraction technique of choice for Cannabis-based preparations and products in recent years [25,28,29]. Our protocol is based on Merck technical reports [31,32].…”

Section: Resultsmentioning

confidence: 99%

“…A blank with the olive oil used for trapping the volatiles and cannabinoid extraction was prepared and analyzed under the same conditions to verify that its oil aromatic profile did not interfere with the retention times of the IS (14.93 min, Figure 2) and Cannabis terpenes (between 4 and 9 min for monoterpenes, 9 and 12 min for monoterpenoids, 17 and 21 min for sesquiterpenes and 22 and 24 min for sesquiterpenoids; Figure 2 and Table 1). As outlined in the first paragraph, HS-SPME has been considered the analytical extraction technique of choice for Cannabis-based preparations and products in recent years [25,28,29]. Our protocol is based on Merck technical reports [31,32].…”

Section: Resultsmentioning

confidence: 99%

“…The combination of mass spectrometry (MS) and chromatographic separation can considerably improve the efficiency of the analytical method [ 24 ]. The use of automated sample preparation methods, such as static headspace (SHS) [ 8 , 25 ] and solid-phase microextraction (SPME) [ 25 , 26 ], means that the extraction step can be avoided and can reduce or eliminate sample incompatibility with the analytical systems, limit matrix interference, while also, more importantly, concentrating the samples [ 27 ].…”

Section: Introductionmentioning

confidence: 99%

“…If the injection of HS does not reach adequate sensitivity, analytes can be directly extracted and concentrated onto sorbent polymers, which may improve detection limits, while integrating sampling, extraction, concentration and sample introduction into a single solvent-free step. HS-SPME is an emerging analytical extraction technique for the sample preparation of Cannabis -based products, and several papers [ 25 , 28 , 29 ] and technical reports [ 26 , 30 , 31 , 32 , 33 , 34 ] have described SPME as an extraction method for the analysis of this plant.…”

Section: Introductionmentioning

confidence: 99%

“…A study on different SPME fibers (CAR-PDMS, PDMS, PDMS-DVB or divinylbenzene, CAR-PDMS-DVB) demonstrated that DVB/CAR/PDMS was able to extract a higher amount of terpenes than the others [ 29 ], confirmed also by other reports [ 31 , 32 , 34 ]. In a recent work, Giovannoni et al reported that extraction efficiencies were higher when using 50/30 μm DVB/CAR/PDMS fibers, especially for more volatile compounds (monoterpenes), but the 30 μm PDMS fiber allowed them to obtain larger peak heights for sesquiterpenes, avoiding the saturation of monoterpene signals [ 25 ].…”

Section: Introductionmentioning

confidence: 99%

See 4 more Smart Citations

Efficient Capture of Cannabis Terpenes in Olive Oil during Microwave-Assisted Cannabinoid Decarboxylation

Boffa,

Binello,

Cravotto

2024

Molecules

View full text Add to dashboard Cite

The development of selective extraction protocols for Cannabis-inflorescence constituents is still a significant challenge. The characteristic Cannabis fragrance can be mainly ascribed to monoterpenes, sesquiterpenes and oxygenated terpenoids. This work investigates the entrapment of Cannabis terpenes in olive oil from inflorescences via stripping under mild vacuum during the rapid microwave-assisted decarboxylation of cannabinoids (MW, 120 °C, 30 min) and after subsequent extraction of cannabinoids (60 and 100 °C). The profiles of the volatiles collected in the oil samples before and after the extraction step were evaluated using static headspace solid-phase microextraction (HS-SPME), followed by gas chromatography coupled to mass spectrometry (GC-MS). Between the three fractions obtained, the first shows the highest volatile content (~37,400 mg/kg oil), with α-pinene, β-pinene, β-myrcene, limonene and trans-β-caryophyllene as the main components. The MW-assisted extraction at 60 and 100 °C of inflorescences using the collected oil fractions allowed an increase of 70% and 86% of total terpene content, respectively. Considering the initial terpene amount of 91,324.7 ± 2774.4 mg/kg dry inflorescences, the percentage of recovery after decarboxylation was close to 58% (mainly monoterpenes), while it reached nearly 100% (including sesquiterpenes) after extraction. The selective and efficient extraction of volatile compounds, while avoiding direct contact between the matrix and extraction solvents, paves the way for specific applications in various aromatic plants. In this context, aromatized extracts can be employed to create innovative Cannabis-based products within the hemp processing industry, as well as in perfumery, cosmetics, dietary supplements, food, and the pharmaceutical industry.

show abstract

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Efficient Capture of Cannabis Terpenes in Olive Oil during Microwave-Assisted Cannabinoid Decarboxylation

Boffa,

Binello,

Cravotto

2024

Molecules

View full text Add to dashboard Cite

show abstract

Simultaneous quantification of terpenes and cannabinoids by reversed-phase LC-APCI-MS/MS in Cannabis sativa L. samples combined with a subsequent chemometric analysis

Raeber,

Poetzsch,

Schmidli

et al. 2024

Anal Bioanal Chem

View full text Add to dashboard Cite

Cannabis sativa L. has been the most discussed medicinal plant in recent years. In particular, the dynamic shift from a formerly illicit and tightly controlled substance to a plant recognized for both medicinal and recreational purposes has brought C. sativa into the global spotlight. Due to the ongoing international legalization processes, fast and convenient analytical methods for the quality control of C. sativa flowers for medicinal and recreational purposes are of tremendous interest. In this study, we report the development and validation of a liquid chromatography-tandem mass spectrometry (LC–MS/MS)-based method applying atmospheric pressure chemical ionization (APCI) to fully quantify 16 terpenes and 7 cannabinoids including their acidic forms by a single chromatographic method. The method presented here is unique and simple, as it eliminates the need for derivatization reactions and includes the unconventional analysis of volatile compounds by liquid chromatography. Samples were prepared by a simple and fast ethanolic extraction. Separation was accomplished within 25 min on a reversed-phase C18 column. Method validation was conducted according to international guidelines regarding selectivity, accuracy, precision, robustness, and linearity. Detection was done in multiple reaction monitoring, which allowed the simultaneous quantification of co-eluting analytes applying two selective mass transitions. In addition, due to reproducible in-source decarboxylation, the acidic forms of cannabinoids were reliably quantified using mass transitions of the neutral forms. The accuracy given as the bias was below 15% for all analytes. Matrix effects for cannabinoids were studied by spiking Humulus lupulus extracts with the analytes at varying concentrations. APCI did not show susceptibility toward ion suppression or enhancement. In addition, the recovery effect after spiking was between 80 and 120% for terpenes. Further, 55 authentic C. sativa extracts were fully quantified, and the obtained results for the terpene profiles were compared to state-of-the-art gas chromatography coupled to flame ionization detection. Comparable results were achieved, emphasizing the method’s applicability for cannabinoids and terpenes. Further, acquired metabolite patterns for C. sativa samples were studied, identifying a relationship between cannabinoid and terpene patterns, as well as the abundance of myrcene in CBD-dominant C. sativa strains. Graphical Abstract

show abstract

Determination of gas-polydimethylsiloxane distribution constants of major Cannabis terpenes and terpenoids by capillary gas-liquid chromatography

Giovannoni

Critto

Lancioni

et al. 2023

Journal of Chromatography A

View full text Add to dashboard Cite

Determination of variability of terpenes and terpenoids in Cannabis sativa by gas chromatography-flame ionization detection and gas chromatography-mass spectrometry

Cited by 9 publications

References 19 publications

Efficient Capture of Cannabis Terpenes in Olive Oil during Microwave-Assisted Cannabinoid Decarboxylation

Efficient Capture of Cannabis Terpenes in Olive Oil during Microwave-Assisted Cannabinoid Decarboxylation

Simultaneous quantification of terpenes and cannabinoids by reversed-phase LC-APCI-MS/MS in Cannabis sativa L. samples combined with a subsequent chemometric analysis

Determination of gas-polydimethylsiloxane distribution constants of major Cannabis terpenes and terpenoids by capillary gas-liquid chromatography

Contact Info

Product

Resources

About