Novel Liquid Chromatography–Tandem Mass Spectrometry Method for Analysis of 102 Pesticides and Five Mycotoxins Regulated by the State of Colorado in Dried Hemp

Abstract

A novel liquid chromatography–tandem mass spectrometry (LC–MS/MS) method with a dual electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) source was developed for analyzing 102 pesticides and five mycotoxins that are regulated by the state of Colorado in hemp. The limit of quantitation (LOQ) of the 102 pesticides and five mycotoxins met Colorado state action limit requirements for these analytes in a hemp matrix. For this study, 88 out of 102 pesticides and all five mycotoxins were analyzed using LC–MS/MS with an ESI source, whereas the remaining 14 pesticides were determined using LC–MS/MS with an APCI source. A simple, fast, green, and cheap acetonitrile solvent extraction method was used to extract the pesticides and mycotoxins from the hemp matrix with good extraction efficiency in the range of 80–120%. A hemp matrix is challenging and causes matrix effects such as ion suppression or enhancement. We optimized the LC method and added 30 internal standards to reduce and compensate for these matrix effects to obtain method accuracy in the range of 70–120%. The ionization mechanism of nonpolar pesticides (normally analyzed by gas chromatography–tandem mass spectrometry [GC–MS/MS]) with an APCI ion source was elucidated.