Evaluation of Three Multiresidue Methods for the Determination of Pesticides in Marijuana (Cannabis sativa L.) with Liquid Chromatography-Tandem Mass Spectrometry

Abstract

Marijuana (non-medical cannabis) is a well-recognized psychoactive herbal drug used for recreational purposes. The aim of this work is to describe and compare the performance and suitability of selected methods to analyze pesticide residues in marijuana. The fitness of three typical pesticide multiresidue methods [acetate buffered QuEChERS (method A), a modified citrate buffered QuEChERS (method B) and citrate buffered QuEChERS (method C)] were tested in marijuana through the LC–MS/MS determination of 61 LC amenable pesticides. Considering recoveries at the highest level for the selected pesticides in marijuana, from the 61 target analytes, 37 (method A), 40 (method B) and 46 (method C) compounds gave accurate results (70–120 % range). Method C showed the best performance for the target analytes in terms of recoveries, precision, limits of quantitation and matrix effect. Marijuana showed to be a highly complex matrix. Most analytes suffered high signal suppression (ME <−50 %) for method B while medium (−50 to 20 %) to low (−20 to 0 %) signal suppression was found for methods A and C. Moreover, high coelution of coextractives with the target analytes was observed. A pilot survey with real samples revealed that seized and legally produced marijuana samples contained pesticides. Residues of diazinon (0.03 mg kg−1), tebuconazole (0.19 mg kg−1) and teflubenzuron (0.11 mg kg−1) were simultaneously detected in one marijuana sample. The establishment of MRLs in a legal consumption scenario such as in Uruguay seems to be necessary in the near future.

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Acknowledgments

Authors acknowledge Polo Agroalimentario y Agroindustrial from Paysandú (PAAP) for their facilities and funding support from PEDECIBA (Programa de Desarrollo de las Ciencias Básicas). Authors specially acknowledge Dr. Carlos García and Mr. Santiago Fernández for their teaching, assistance and remarkable discussions during the time this work has been done.

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Correspondence to Andrés Pérez-Parada.

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Published in the topical collection 5th Latin American Pesticide Residue Workshop with guest editor Steven J. Lehotay.

An erratum to this article is available at http://dx.doi.org/10.1007/s10337-016-3130-0.

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Pérez-Parada, A., Alonso, B., Rodríguez, C. et al. Evaluation of Three Multiresidue Methods for the Determination of Pesticides in Marijuana (Cannabis sativa L.) with Liquid Chromatography-Tandem Mass Spectrometry. Chromatographia 79, 1069–1083 (2016). https://doi.org/10.1007/s10337-016-3029-9

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Keywords

  • Pesticide residues
  • LC–MS/MS
  • Mass spectrometry
  • QuEChERS
  • Marijuana
  • Cannabis