Validation of a high-throughput method for analysis of pesticide residues in hemp and hemp products

Michlig, Nicolás; Lehotay, Steven J.; Beldoménico, Horacio; Repetti, María Rosa

doi:10.1016/j.chroma.2021.462097

Cited by 23 publications

(25 citation statements)

References 39 publications

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“…Separation of contaminants was carried out by chromatographic techniques, either by GC or LC, but the latter one was used to a greater extent, due to its versatility and capacity to analyze semi-polar and polar pesticides, 42 which are commonly used in cannabis plantations. GC was employed to analyze pesticide residues in cannabis oil, dried cannabis flowers and cannabis leaves, employing a TR-pesticide II capillary column, 25 while the capillary column HP-5 ms was used to determine pesticides in cress, fennel, flax, and hemp seeds, 35 cannabis plantations, 23 hemp and hemp products 37 and cannabis smoke 40 (Table 2).…”

Section: Separation and Detectionmentioning

confidence: 99%

“…27 Acetonitrile was also used as extraction solvent to simultaneously extract pesticides and mycotoxins in cannabis, and extracts were filtered before determination, and recoveries ranged from 70% to 120%. 36 Finally, Michlig et al 37 developed a QuEChERSER method (quick, easy, cheap, effective, rugged, safe, efficient, and robust), employing acetonitrile with water (4:1, v/v) to extract pesticides and metabolites from hemp and hemp products. Recoveries ranged from 24% to 153% for the 93 pesticides and metabolites, with 80-90% of them in the acceptance range (70-120%).…”

mentioning

confidence: 99%

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Recent applications of chromatography for analysis of contaminants in cannabis products: a review

López‐Ruiz¹,

Marín-Sáez²,

Frenich³

2021

Pest Management Science

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In the last few years, the cultivation of cannabis has been increasing due to greater use in foods, recreational use, creams, oils, and other applications. Thus, analysis of contaminants (e.g. pesticides and mycotoxins) in cannabis products is necessary to ensure consumer safety. This review is focused on the analytical procedures, based on chromatographic techniques, used for the determination of contaminants in cannabis and related products, developed from 2015 to 2020. QuEChERS (acronym of quick, easy, cheap, effective, rugged and safe) was mainly used for the extraction of pesticides and other contaminants from cannabis because its versatility and capacity to extract a wide range of substances, and therefore, increasing the scope of the analysis. The most employed technique to determine pesticides and mycotoxins in cannabis products was liquid chromatography (LC) coupled to mass spectrometry (MS), although gas chromatography (GC) coupled to MS was also employed for the analysis of non-polar compounds, using triple quadrupole (QqQ) as mass analyzer. Nevertheless, new advances in cannabis analysis are also discussed, introducing techniques such as high-resolution mass spectrometry (HRMS), which allows for performing both targeted and untargeted (unknown and suspect) analyses.

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Section: Separation and Detectionmentioning

confidence: 99%

mentioning

confidence: 99%

Recent applications of chromatography for analysis of contaminants in cannabis products: a review

López‐Ruiz¹,

Marín-Sáez²,

Frenich³

2021

Pest Management Science

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“…Relevant studies seeking to address the need of reliable testing methods in cannabis and its derived products have been published over the last years [ 3 , 4 , 5 , 6 , 7 , 8 , 9 ]. With regards to pesticides testing, the great majority of the works have been focused on plant material [ 4 , 5 , 6 , 10 ], followed by some studies on cannabis oils [ 11 , 12 , 13 ]. It is worth mentioning that a stake holder panel on strategic food analytical methods recently published in the Journal of the Association of Official Analytical Chemists (AOAC), a set of standard method performance requirements (SMPRs) describing the minimum recommended performance criteria for any method to be applied in the analysis of pesticides in dried cannabis [ 14 ].…”

Section: Introductionmentioning

confidence: 99%

“…Common sample preparation strategies for the isolation of pesticides from diverse cannabis products involve solvent extraction followed by extract dilution; QuEChERS; and SPE as an extract clean‐up step [ 6 , 11 , 15 , 16 , 17 , 18 ]. An updated version of QuEChERS known as QuEChERSER mega method, which stands for quick, easy, cheap, effective, rugged, safe, efficient, and robust, was recently applied for the analysis of a broad range of pesticides in hemp matrices [ 10 ]. Other approaches involving SPME and direct coupling of SPME‐based devices with tandem mass spectrometry (MS/MS) have also been evaluated, and satisfactory results have been found for a limited number pesticides [ 12 , 19 ].…”

Section: Introductionmentioning

confidence: 99%

“…Under these conditions, faster separations can be attained while maintaining the same degree of resolution [ 20 , 23 ]. It should be noted that LPGC‐MS/MS was recently used for the determination of multiple GC amenable pesticides regulated by USA and Canada in hemp products extracts obtained via QuEChERSER and after automated robotic minicolumn SPE cleanup [ 10 ]. The results of this study demonstrated the potential of LPGC‐MS/MS for faster analysis of GC‐amenable contaminants in cannabis products.…”

Section: Introductionmentioning

confidence: 99%

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Analysis of the California list of pesticides, mycotoxins, and cannabinoids in chocolate using liquid chromatography and low‐pressure gas chromatography‐based platforms

Reyes‐Garcés

Myers

2021

J of Separation Science

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Cannabis legalization has led to the development of a variety of cannabis-infused products with edibles being one of the most popular. The state of California has implemented comprehensive cannabis testing regulations requiring the analysis of cannabinoids (potency) and contaminants, such as pesticides and mycotoxins, in any type of cannabis good. In this work, we propose an analytical workflow for the quantification of the California list of pesticides and mycotoxins, as well as six cannabinoids, in chocolate, using 3 mL of solvent for the extraction. For the analysis of pesticides and mycotoxins, clean-up steps employing a C18 solidphase extraction cartridge and dispersive solid-phase extraction sorbents were implemented. Gas chromatography amenable pesticides were analyzed using low-pressure gas chromatography coupled to tandem mass spectrometry which allowed for a total method run of 12 min. Both liquid chromatography and gas chromatography instrumental methods had the same analysis time, ensuring satisfactory sample throughput. For the determination of cannabinoids, a dilution of the original organic extract collected for pesticides and mycotoxins analysis (and prior to any clean-up step) was used. Excellent results in terms of analytical figures of merit were obtained for all target analytes.

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A dilute‐and‐inject low‐pressure gas chromatography‐tandem mass spectrometry method for phthalate determination in extra virgin olive oil

Ferracane,

Zoccali,

Arena

et al. 2023

J of Separation Science

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The goal of this study was to develop a method for the determination of nine phthalic acid esters in extra virgin olive oils using low‐pressure gas chromatography‐triple‐quadrupole mass spectrometry. Sample preparation was simple, environmental friendly, and rapid inasmuch that it involved only dilution (< 1 mL of hexane). The low‐pressure gas chromatography analyses were performed by using a 5 m wide‐bore column. The limit of quantification for the phthalates ranged from 0.06 to 1.14 mg kg−1. Both intra‐ and interday precisions were measured, with coefficient of variation values ranging from 0.2% to 11.7%. The trueness of the method was measured by evaluating accuracy at the initial stage of the work and after 2 months, with values ranging between −8.7% and 12.1%. Moreover, blind accuracy was comprised between −11.6% and 14.2%. The method involves the use of simplified instrumentation and reduced analysis times (nearly two times faster) compared to a previously published comprehensive two‐dimensional gas chromatography‐triple‐quadrupole mass spectrometry method, leading to a reduction of energy and helium consumption. The approaches were compared in analytical terms and for the environmental impact. In total, 23 olive oil samples were analyzed, with at least one phthalate detected in all but one sample.

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Validation of a high-throughput method for analysis of pesticide residues in hemp and hemp products

Cited by 23 publications

References 39 publications

Recent applications of chromatography for analysis of contaminants in cannabis products: a review

Recent applications of chromatography for analysis of contaminants in cannabis products: a review

Analysis of the California list of pesticides, mycotoxins, and cannabinoids in chocolate using liquid chromatography and low‐pressure gas chromatography‐based platforms

A dilute‐and‐inject low‐pressure gas chromatography‐tandem mass spectrometry method for phthalate determination in extra virgin olive oil

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