Multiresidue Determination of Pesticides in Malt Beverages by Capillary Gas Chromatography with Mass Spectrometry and Selected Ion Monitoring

Abstract

A method was developed to determine pesticides in malt beverages using solid phase extraction on a polymeric cartridge and sample cleanup with a MgSO4-topped aminopropyl cartridge, followed by capillary gas chromatography with electron impact mass spectrometry in the selected ion monitoring mode [GC-MS(SIM)]. Three GC injections were required to analyze and identify organophosphate, organohalogen, and organonitrogen pesticides. The pesticides were identified by the retention times of peaks of the target ion and qualifier-to-target ion ratios. GC detection limits for most of the pesticides were 5-10 ng/mL, and linearity was determined from 50 to 5000 ng/mL. Fortification studies were performed at 10 ng/mL for three malt beverages that differ in properties such as alcohol content, solids, and appearance. The recoveries from the three malt beverages were greater than 70% for 85 of the 142 pesticides (including isomers) studied. The data showed that the different malt beverage matrixes had no significant effect on the recoveries. This method was then applied to the screening and analysis of malt beverages for pesticides, resulting in the detection of the insectide carbaryl and the fungicide dimethomorph in real samples. The study indicates that pesticide levels in malt beverages are significantly lower than the tolerance levels set by the United States Environmental Protection Agency for malt beverage starting ingredients. The use of the extraction/cleanup procedure and analysis by GC-MS(SIM) proved effective in screening malt beverages for a wide variety of pesticides.

Functionalized inorganic nanoparticles used as labels in solid-phase immunoassays

“…However, the mean recovery values assayed in this work are in the same order of magnitude than those found in previous works for most water and food samples considered [7,11,13,14]. Concerning to the LODs, our values were better or of the same order that those reported using either SPE with conventional cartridges [1,6] or liquid-liquid extraction [13]. However, the LODs achieved in this work were comparable to the ones obtained by Yang et al [14].…”

“…The distinct features of these multirresidual analytical methods are summarized in Table 3. As can be seen, some works for certain food matrices showed low recoveries for CLT (< 70%) [6,[8][9][10]12]. However, the mean recovery values assayed in this work are in the same order of magnitude than those found in previous works for most water and food samples considered [7,11,13,14].…”

Salting-out Assisted Liquid-Liquid Extraction for the Determination of Multiresidue Pesticides in Alcoholic Beverages by High Performance Liquid Chromatography

“…Nevertheless, their wide use in or on agricultural products might be resulted in the occurrence of residues of these chemicals and their metabolites in raw as well as processed food commodities, water and soil [1]. Alcoholic beverages which are usually prepared from various agricultural products and are considered as a part of human diet [2] could also be directly or indirectly contaminated by these pesticides and subsequently, could affect the health of consumers [3][4][5][6][7][8][9]. To monitor and control the health of consumers, legislative authorities and monitoring organizations of different countries, have set maximum residue limits (MRLs) of pesticide residues in various raw and processed foods, including alcoholic beverages [9][10][11][12].…”

“…Gas chromatography (GC) with various detectors including flame ionization detector (FID) [13,14], electron capture (ECD) [15], nitrogen-phosphorus detection (NPD) [15,16], mass spectrometric detector (MS) [7,8,17], tandem mass spectrometry (MS/MS) [5], capillary liquid chromatography coupled with diode array detection (cHPLC-DAD) [3], ultra-high pressure liquid chromatography coupled to MS/MS (UHPLC-MS/MS) [4] and liquid chromatography with MS/MS (LC-MS/MS) [18] have been used for determination of pesticides residues in wine. UHPLC-MS/MS [4], GC-ECD, GC-MS [19] and LC-MS/MS [20] were reported for determination of pesticide residues in beer [20].…”

“…In spite of its numerous disadvantages, such as time consuming, labor intensiveness, use of large sample size and high volumes of expensive and hazardous organic solvents, solid-phase extraction (SPE) [7,8,17,18] has been widely used for extraction and/or preconcentration of pesticide residues from alcoholic beverages. Solid-phase microextraction (SPME) [5] has also been reported for extraction of pesticides from wine.…”