Modeling a pesticide remediation strategy for preparative liquid chromatography using high-performance liquid chromatography
Abstract Background Cannabis sativa L. also known as industrial hemp, is primarily cultivated as source material for cannabinoids cannabidiol (CBD) and ∆9-tetrahydrocannabinol (∆9-THC). Pesticide contamination during plant growth is a common issue in the cannabis industry which can render plant biom...
| Main Authors: | , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
BMC
2023-04-01
|
| Series: | Journal of Cannabis Research |
| Subjects: | |
| Online Access: | https://doi.org/10.1186/s42238-023-00172-1 |
| _version_ | 1797845843266502656 |
|---|---|
| author | Jamie Cuchiaro James Baumgartner Melissa M. Reynolds |
| author_facet | Jamie Cuchiaro James Baumgartner Melissa M. Reynolds |
| author_sort | Jamie Cuchiaro |
| collection | DOAJ |
| description | Abstract Background Cannabis sativa L. also known as industrial hemp, is primarily cultivated as source material for cannabinoids cannabidiol (CBD) and ∆9-tetrahydrocannabinol (∆9-THC). Pesticide contamination during plant growth is a common issue in the cannabis industry which can render plant biomass and products made from contaminated material unusable. Remediation strategies to ensure safety compliance are vital to the industry, and special consideration should be given to methods that are non-destructive to concomitant cannabinoids. Preparative liquid chromatography (PLC) is an attractive strategy for remediating pesticide contaminants while also facilitating targeted isolation cannabinoids in cannabis biomass. Methods The present study evaluated the benchtop-scale suitability of pesticide remediation by liquid chromatographic eluent fractionation, by comparing retention times of 11 pesticides relative to 26 cannabinoids. The ten pesticides evaluated for retention times are clothianidin, imidacloprid, piperonyl butoxide, pyrethrins (I/II mixture), diuron, permethrin, boscalid, carbaryl, spinosyn A, and myclobutanil. Analytes were separated prior to quantification on an Agilent Infinity II 1260 high performance liquid chromatography with diode array detection (HPLC-DAD). The detection wavelengths used were 208, 220, 230, and 240 nm. Primary studies were performed using an Agilent InfinityLab Poroshell 120 EC-C18 3.0 × 50 mm column with 2.7 μm particle diameter, using a binary gradient. Preliminary studies on Phenomenex Luna 10 μm C18 PREP stationary phase were performed using a 150 × 4.6 mm column. Results The retention times of standards and cannabis matrices were evaluated. The matrices used were raw cannabis flower, ethanol crude extract, CO2 crude extract, distillate, distillation mother liquors, and distillation bottoms. The pesticides clothianidin, imidacloprid, carbaryl, diuron, spinosyn A, and myclobutanil eluted in the first 3.6 min, and all cannabinoids (except for 7-OH-CBD) eluted in the final 12.6 min of the 19-minute gradient for all matrices evaluated. The elution times of 7-OH-CBD and boscalid were 3.44 and 3.55 min, respectively. Discussion 7-OH-CBD is a metabolite of CBD and was not observed in the cannabis matrices evaluated. Thus, the present method is suitable for separating 7/11 pesticides and 25/26 cannabinoids tested in the six cannabis matrices tested. 7-OH-CBD, pyrethrins I and II (RTA: 6.8 min, RTB: 10.5 min), permethrin (RTA: 11.9 min, RTB: 12.2 min), and piperonyl butoxide (RTA: 8.3 min, RTB: 11.7 min), will require additional fractionation or purification steps. Conclusions The benchtop method was demonstrated have congruent elution profiles using preparative-scale stationary phase. The resolution of pesticides from cannabinoids in this method indicates that eluent fractionation is a highly attractive industrial solution for pesticide remediation of contaminated cannabis materials and targeted isolation of cannabinoids. |
| first_indexed | 2024-04-09T17:45:30Z |
| format | Article |
| id | doaj.art-e8f699bb92b446ce9e99c501d02a53be |
| institution | Directory Open Access Journal |
| issn | 2522-5782 |
| language | English |
| last_indexed | 2024-04-09T17:45:30Z |
| publishDate | 2023-04-01 |
| publisher | BMC |
| record_format | Article |
| series | Journal of Cannabis Research |
| spelling | doaj.art-e8f699bb92b446ce9e99c501d02a53be2023-04-16T11:24:07ZengBMCJournal of Cannabis Research2522-57822023-04-01511910.1186/s42238-023-00172-1Modeling a pesticide remediation strategy for preparative liquid chromatography using high-performance liquid chromatographyJamie Cuchiaro0James Baumgartner1Melissa M. Reynolds2Department of Chemistry, Colorado State UniversityPanacea Life SciencesDepartment of Chemistry, Colorado State UniversityAbstract Background Cannabis sativa L. also known as industrial hemp, is primarily cultivated as source material for cannabinoids cannabidiol (CBD) and ∆9-tetrahydrocannabinol (∆9-THC). Pesticide contamination during plant growth is a common issue in the cannabis industry which can render plant biomass and products made from contaminated material unusable. Remediation strategies to ensure safety compliance are vital to the industry, and special consideration should be given to methods that are non-destructive to concomitant cannabinoids. Preparative liquid chromatography (PLC) is an attractive strategy for remediating pesticide contaminants while also facilitating targeted isolation cannabinoids in cannabis biomass. Methods The present study evaluated the benchtop-scale suitability of pesticide remediation by liquid chromatographic eluent fractionation, by comparing retention times of 11 pesticides relative to 26 cannabinoids. The ten pesticides evaluated for retention times are clothianidin, imidacloprid, piperonyl butoxide, pyrethrins (I/II mixture), diuron, permethrin, boscalid, carbaryl, spinosyn A, and myclobutanil. Analytes were separated prior to quantification on an Agilent Infinity II 1260 high performance liquid chromatography with diode array detection (HPLC-DAD). The detection wavelengths used were 208, 220, 230, and 240 nm. Primary studies were performed using an Agilent InfinityLab Poroshell 120 EC-C18 3.0 × 50 mm column with 2.7 μm particle diameter, using a binary gradient. Preliminary studies on Phenomenex Luna 10 μm C18 PREP stationary phase were performed using a 150 × 4.6 mm column. Results The retention times of standards and cannabis matrices were evaluated. The matrices used were raw cannabis flower, ethanol crude extract, CO2 crude extract, distillate, distillation mother liquors, and distillation bottoms. The pesticides clothianidin, imidacloprid, carbaryl, diuron, spinosyn A, and myclobutanil eluted in the first 3.6 min, and all cannabinoids (except for 7-OH-CBD) eluted in the final 12.6 min of the 19-minute gradient for all matrices evaluated. The elution times of 7-OH-CBD and boscalid were 3.44 and 3.55 min, respectively. Discussion 7-OH-CBD is a metabolite of CBD and was not observed in the cannabis matrices evaluated. Thus, the present method is suitable for separating 7/11 pesticides and 25/26 cannabinoids tested in the six cannabis matrices tested. 7-OH-CBD, pyrethrins I and II (RTA: 6.8 min, RTB: 10.5 min), permethrin (RTA: 11.9 min, RTB: 12.2 min), and piperonyl butoxide (RTA: 8.3 min, RTB: 11.7 min), will require additional fractionation or purification steps. Conclusions The benchtop method was demonstrated have congruent elution profiles using preparative-scale stationary phase. The resolution of pesticides from cannabinoids in this method indicates that eluent fractionation is a highly attractive industrial solution for pesticide remediation of contaminated cannabis materials and targeted isolation of cannabinoids.https://doi.org/10.1186/s42238-023-00172-1CannabisCannabinoidsPesticide remediationAdsorptive separationHigh-performance liquid chromatographyPreparative Liquid Chromatography |
| spellingShingle | Jamie Cuchiaro James Baumgartner Melissa M. Reynolds Modeling a pesticide remediation strategy for preparative liquid chromatography using high-performance liquid chromatography Journal of Cannabis Research Cannabis Cannabinoids Pesticide remediation Adsorptive separation High-performance liquid chromatography Preparative Liquid Chromatography |
| title | Modeling a pesticide remediation strategy for preparative liquid chromatography using high-performance liquid chromatography |
| title_full | Modeling a pesticide remediation strategy for preparative liquid chromatography using high-performance liquid chromatography |
| title_fullStr | Modeling a pesticide remediation strategy for preparative liquid chromatography using high-performance liquid chromatography |
| title_full_unstemmed | Modeling a pesticide remediation strategy for preparative liquid chromatography using high-performance liquid chromatography |
| title_short | Modeling a pesticide remediation strategy for preparative liquid chromatography using high-performance liquid chromatography |
| title_sort | modeling a pesticide remediation strategy for preparative liquid chromatography using high performance liquid chromatography |
| topic | Cannabis Cannabinoids Pesticide remediation Adsorptive separation High-performance liquid chromatography Preparative Liquid Chromatography |
| url | https://doi.org/10.1186/s42238-023-00172-1 |
| work_keys_str_mv | AT jamiecuchiaro modelingapesticideremediationstrategyforpreparativeliquidchromatographyusinghighperformanceliquidchromatography AT jamesbaumgartner modelingapesticideremediationstrategyforpreparativeliquidchromatographyusinghighperformanceliquidchromatography AT melissamreynolds modelingapesticideremediationstrategyforpreparativeliquidchromatographyusinghighperformanceliquidchromatography |