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==Abstract== | ==Abstract== | ||
A method has been developed to screen [[Cannabis concentrate|cannabis extracts]] for more than 1,000 [[pesticide]]s and environmental pollutants using [[gas chromatography] coupled to a high-resolution accurate mass [[quadrupole]] [[Time-of-flight mass spectrometry|time-of-flight mass spectrometer]] (GC/Q-TOF). An extraction procedure was developed using [[wikipedia:Acetonitrile|acetonitrile]] with [[solid-phase extraction]] cleanup. Before analysis, extracts were diluted 125:1 with [[solvent]]. Two data mining approaches were used together with a retention-time-locked Personal Compound Database and Library (PCDL) containing high-resolution accurate [[Mass spectrometry|mass spectra]] for pesticides and other environmental pollutants. In the first approach, a Find-by-Fragments (FbF) software tool extracted several characteristic exact mass ions within a small retention time window where the compound [[Elution|eluted]]. For each compound in the PCDL, the software evaluated the peak shape and retention time of each ion, as well as the monoisotopic exact mass, ion ratios, and other factors to decide if the compound was present or not. In the second approach, Unknowns Analysis (UA) software with a peak-finding algorithm called SureMass was used to deconvolute peaks in the [[Chromatography|chromatogram]]. The accurate mass spectra were searched against the PCDL using spectral matching and retention time as filters. A subset PCDL was generated containing only pesticides that are most likely to be found on foods in the US. With about 250 compounds in the smaller PCDL, there were fewer hits for non-pesticides, and data review was much faster. Organically grown [[cannabis]] was used for method development. Twenty-one confiscated cannabis [[Sample (material)|samples]] were analyzed and ten were found to have no detectable pesticides. The remaining 11 samples had at least one pesticide, and one sample had seven detectable residues. Quantitative analysis was run on the confiscated samples for a subset of the pesticides found by screening. Two cannabis samples had residues of [[carbaryl]] and [[malathion]] that were estimated to be about 10 times greater than the highest [[United States Environmental Protection Agency|U.S. Environmental Protection Agency]] (EPA) tolerance set for food and about 4,000 times greater than the Canadian maximum residue limits for dried cannabis [[Inflorescence|flower]]. | A method has been developed to screen [[Cannabis concentrate|cannabis extracts]] for more than 1,000 [[pesticide]]s and environmental pollutants using [[gas chromatography]] coupled to a high-resolution accurate mass [[quadrupole]] [[Time-of-flight mass spectrometry|time-of-flight mass spectrometer]] (GC/Q-TOF). An extraction procedure was developed using [[wikipedia:Acetonitrile|acetonitrile]] with [[solid-phase extraction]] cleanup. Before analysis, extracts were diluted 125:1 with [[solvent]]. Two data mining approaches were used together with a retention-time-locked Personal Compound Database and Library (PCDL) containing high-resolution accurate [[Mass spectrometry|mass spectra]] for pesticides and other environmental pollutants. In the first approach, a Find-by-Fragments (FbF) software tool extracted several characteristic exact mass ions within a small retention time window where the compound [[Elution|eluted]]. For each compound in the PCDL, the software evaluated the peak shape and retention time of each ion, as well as the monoisotopic exact mass, ion ratios, and other factors to decide if the compound was present or not. In the second approach, Unknowns Analysis (UA) software with a peak-finding algorithm called SureMass was used to deconvolute peaks in the [[Chromatography|chromatogram]]. The accurate mass spectra were searched against the PCDL using spectral matching and retention time as filters. A subset PCDL was generated containing only pesticides that are most likely to be found on foods in the US. With about 250 compounds in the smaller PCDL, there were fewer hits for non-pesticides, and data review was much faster. Organically grown [[cannabis]] was used for method development. Twenty-one confiscated cannabis [[Sample (material)|samples]] were analyzed and ten were found to have no detectable pesticides. The remaining 11 samples had at least one pesticide, and one sample had seven detectable residues. Quantitative analysis was run on the confiscated samples for a subset of the pesticides found by screening. Two cannabis samples had residues of [[carbaryl]] and [[malathion]] that were estimated to be about 10 times greater than the highest [[United States Environmental Protection Agency|U.S. Environmental Protection Agency]] (EPA) tolerance set for food and about 4,000 times greater than the Canadian maximum residue limits for dried cannabis [[Inflorescence|flower]]. | ||
==Introduction== | ==Introduction== | ||
The use of [[Cannabis (drug)|medicinal cannabis]] is legal in 20 countries and 33 U.S. states, while two countries, Canada and Uruguay, have fully [[Legality of cannabis|legalized]] the sale and use of recreational [[cannabis]] nationwide.<ref name="HassanWhere18">{{cite web |url=https://qz.com/1427177/where-is-marijuana-legal-around-the-world/ |title=All the places in the world you can (legally) smoke weed |author=Hassan, A. |work=Quartz |date=17 October 2018 |accessdate=01 May 2019}}</ref> In the U.S., 11 states and the District of Columbia have legalized recreational use of cannabis, but it is still illegal at the federal level. Many countries and U.S. states have decriminalized possession and use of cannabis.<ref name="DISAMap19">{{cite web |url=https://disa.com/map-of-marijuana-legality-by-state |title=Map of Marijuana Legality by State |publisher=DISA Global Solutions |date=2019 |accessdate=01 May 2019}}</ref> With so many people having access to cannabis, there is an increased need to [[RefWork:Past, Present, and Future of Cannabis Laboratory Testing and Regulation in the United States|test cannabis]] products to ensure their safety. ''Cannabis'' plants are subject to various pests and diseases which may require the judicious use of [[pesticide]]s to maintain plant health. McPartland has published two comprehensive reviews on the diseases<ref name="McPartlandARev96">{{cite journal |title=A review of ''Cannabis'' diseases |journal=Journal of the International Hemp Association |author=McPartland, J.M. |volume=3 |issue=1 |pages=19–23 |year=1996 |url=http://www.internationalhempassociation.org/jiha/iha03111.html}}</ref> and pests<ref name="McPartlandCanna96">{{cite journal |title=''Cannabis'' pests |journal=Journal of the International Hemp Association |author=McPartland, J.M. |volume=3 |issue=2 |pages=49, 52–55 |year=1996 |url=http://www.internationalhempassociation.org/jiha/iha03201.html}}</ref> that attack ''Cannabis'' plants. But, pesticide residues on the plant material are particularly concerning because cannabis can be ingested, smoked, or extracted and concentrated for use in everything from food and beverages to tinctures and suppositories. Many jurisdictions that have legalized cannabis require testing for pesticide residues. For example, Oregon<ref name="FarrerTech15">{{cite web |url=https://www.oregon.gov/oha/ph/PreventionWellness/marijuana/Documents/oha-8964-technical-report-marijuana-contaminant-testing.pdf |format=PDF |title=Technical report: Oregon Health Authority’s process to decide which types of contaminants to test for in cannabis products, and levels for action |author=Farrer, D.G. |publisher=Oregon Health Authority |date=December 2015 |accessdate=01 May 2019}}</ref>, California<ref name="TRCCRResid">{{cite web |url=https://govt.westlaw.com/calregs/Document/I8CCCCCCFBE19419D9DDFFA11E5E29042?viewType=FullText&originationContext=documenttoc&transitionType=CategoryPageItem&contextData=(sc.Default)#co_anchor_IB78AA9DD7002490FB0286370F626BEB |title=16 CCR § 5719 Residual Pesticides Testing |work=Westlaw |publisher=Thomson Reuters |accessdate=01 May 2019}}</ref>, and Canada<ref name="GoCMand19">{{cite web |url=https://www.canada.ca/en/public-health/services/publications/drugs-health-products/cannabis-testing-pesticide-list-limits.html |title=Mandatory cannabis testing for pesticide active ingredients - List and limits |author=Health Canada |publisher=Government of Canada |date=2019 |accessdate=01 May 2019}}</ref> have lists of 59, 66, and 95 pesticides, respectively, that must be targeted by analysts. However, some growers use pesticides that are not on lists of acceptable compounds for which maximum residue limits (MRLs) have been set. Product recalls are common, companies have gone out of business, and occasionally, someone is fined for the misuse of pesticides. On top of this, the unregulated market for cannabis is still much bigger than the legal market.<ref name="McGovern11Facts18">{{cite web |url=https://www.greenentrepreneur.com/article/324679 |title=11 Facts Cannabis Entrepreneurs Should Know About the Black Market |author=McGovern, S. |work=Green Entrepreneur |date=17 December 2018 |accessdate=01 May 2019}}</ref> Many of the illegal growers use pesticides carelessly and leave unknown levels of sometimes illegal pesticides on the plant material. One real concern is the affect that pesticides and [[cannabinoid]]s might have on a developing fetus.<ref name="LeungAdverse19">{{cite journal |title=Adverse outcome pathway of developmental neurotoxicity resulting from prenatal exposures to cannabis contaminated with organophosphate pesticide residues |journal=Reproductive Toxicology |author=Leung, M.C.K.; Silva, M.H.; Palumbo, A.J. et al. |volume=85 |pages=12–18 |year=2019 |doi=10.1016/j.reprotox.2019.01.004 |pmid=30668982}}</ref> | |||
==References== | ==References== | ||
Revision as of 17:24, 18 September 2020
| Full article title | Screening for more than 1,000 pesticides and environmental contaminants in cannabis by GC/Q-TOF |
|---|---|
| Journal | Medical Cannabis and Cannabinoids |
| Author(s) | Wylie, P.L.; Westland, J.; Wang, M.; Radwan, M.M.; Majumdat, C.G.; ElSohly, M.A. |
| Author affiliation(s) | Agilent Technologies, University of Mississippi, ElSohly Laboratories |
| Primary contact | Email: Philip dot l dot wylie at gmail dot com |
| Year published | 2020 |
| Volume and issue | 3(1) |
| Page(s) | 14–24 |
| DOI | 10.1159/000504391 |
| ISSN | 2504-3889 |
| Distribution license | Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International |
| Website | https://www.karger.com/Article/FullText/504391 |
| Download | https://www.karger.com/Article/Pdf/504391 (PDF) |
 |
This article should be considered a work in progress and incomplete. Consider this article incomplete until this notice is removed. |
Abstract
A method has been developed to screen cannabis extracts for more than 1,000 pesticides and environmental pollutants using gas chromatography coupled to a high-resolution accurate mass quadrupole time-of-flight mass spectrometer (GC/Q-TOF). An extraction procedure was developed using acetonitrile with solid-phase extraction cleanup. Before analysis, extracts were diluted 125:1 with solvent. Two data mining approaches were used together with a retention-time-locked Personal Compound Database and Library (PCDL) containing high-resolution accurate mass spectra for pesticides and other environmental pollutants. In the first approach, a Find-by-Fragments (FbF) software tool extracted several characteristic exact mass ions within a small retention time window where the compound eluted. For each compound in the PCDL, the software evaluated the peak shape and retention time of each ion, as well as the monoisotopic exact mass, ion ratios, and other factors to decide if the compound was present or not. In the second approach, Unknowns Analysis (UA) software with a peak-finding algorithm called SureMass was used to deconvolute peaks in the chromatogram. The accurate mass spectra were searched against the PCDL using spectral matching and retention time as filters. A subset PCDL was generated containing only pesticides that are most likely to be found on foods in the US. With about 250 compounds in the smaller PCDL, there were fewer hits for non-pesticides, and data review was much faster. Organically grown cannabis was used for method development. Twenty-one confiscated cannabis samples were analyzed and ten were found to have no detectable pesticides. The remaining 11 samples had at least one pesticide, and one sample had seven detectable residues. Quantitative analysis was run on the confiscated samples for a subset of the pesticides found by screening. Two cannabis samples had residues of carbaryl and malathion that were estimated to be about 10 times greater than the highest U.S. Environmental Protection Agency (EPA) tolerance set for food and about 4,000 times greater than the Canadian maximum residue limits for dried cannabis flower.
Introduction
The use of medicinal cannabis is legal in 20 countries and 33 U.S. states, while two countries, Canada and Uruguay, have fully legalized the sale and use of recreational cannabis nationwide.[1] In the U.S., 11 states and the District of Columbia have legalized recreational use of cannabis, but it is still illegal at the federal level. Many countries and U.S. states have decriminalized possession and use of cannabis.[2] With so many people having access to cannabis, there is an increased need to test cannabis products to ensure their safety. Cannabis plants are subject to various pests and diseases which may require the judicious use of pesticides to maintain plant health. McPartland has published two comprehensive reviews on the diseases[3] and pests[4] that attack Cannabis plants. But, pesticide residues on the plant material are particularly concerning because cannabis can be ingested, smoked, or extracted and concentrated for use in everything from food and beverages to tinctures and suppositories. Many jurisdictions that have legalized cannabis require testing for pesticide residues. For example, Oregon[5], California[6], and Canada[7] have lists of 59, 66, and 95 pesticides, respectively, that must be targeted by analysts. However, some growers use pesticides that are not on lists of acceptable compounds for which maximum residue limits (MRLs) have been set. Product recalls are common, companies have gone out of business, and occasionally, someone is fined for the misuse of pesticides. On top of this, the unregulated market for cannabis is still much bigger than the legal market.[8] Many of the illegal growers use pesticides carelessly and leave unknown levels of sometimes illegal pesticides on the plant material. One real concern is the affect that pesticides and cannabinoids might have on a developing fetus.[9]
References
- ↑ Hassan, A. (17 October 2018). "All the places in the world you can (legally) smoke weed". Quartz. https://qz.com/1427177/where-is-marijuana-legal-around-the-world/. Retrieved 01 May 2019.
- ↑ "Map of Marijuana Legality by State". DISA Global Solutions. 2019. https://disa.com/map-of-marijuana-legality-by-state. Retrieved 01 May 2019.
- ↑ McPartland, J.M. (1996). "A review of Cannabis diseases". Journal of the International Hemp Association 3 (1): 19–23. http://www.internationalhempassociation.org/jiha/iha03111.html.
- ↑ McPartland, J.M. (1996). "Cannabis pests". Journal of the International Hemp Association 3 (2): 49, 52–55. http://www.internationalhempassociation.org/jiha/iha03201.html.
- ↑ Farrer, D.G. (December 2015). "Technical report: Oregon Health Authority’s process to decide which types of contaminants to test for in cannabis products, and levels for action" (PDF). Oregon Health Authority. https://www.oregon.gov/oha/ph/PreventionWellness/marijuana/Documents/oha-8964-technical-report-marijuana-contaminant-testing.pdf. Retrieved 01 May 2019.
- ↑ "16 CCR § 5719 Residual Pesticides Testing". Westlaw. Thomson Reuters. https://govt.westlaw.com/calregs/Document/I8CCCCCCFBE19419D9DDFFA11E5E29042?viewType=FullText&originationContext=documenttoc&transitionType=CategoryPageItem&contextData=(sc.Default)#co_anchor_IB78AA9DD7002490FB0286370F626BEB. Retrieved 01 May 2019.
- ↑ Health Canada (2019). "Mandatory cannabis testing for pesticide active ingredients - List and limits". Government of Canada. https://www.canada.ca/en/public-health/services/publications/drugs-health-products/cannabis-testing-pesticide-list-limits.html. Retrieved 01 May 2019.
- ↑ McGovern, S. (17 December 2018). "11 Facts Cannabis Entrepreneurs Should Know About the Black Market". Green Entrepreneur. https://www.greenentrepreneur.com/article/324679. Retrieved 01 May 2019.
- ↑ Leung, M.C.K.; Silva, M.H.; Palumbo, A.J. et al. (2019). "Adverse outcome pathway of developmental neurotoxicity resulting from prenatal exposures to cannabis contaminated with organophosphate pesticide residues". Reproductive Toxicology 85: 12–18. doi:10.1016/j.reprotox.2019.01.004. PMID 30668982.
Notes
This presentation is faithful to the original, with only a few minor changes to presentation. Some grammar and punctuation was cleaned up to improve readability. In some cases important information was missing from the references, and that information was added.
