Simultaneous Determination of 346 Multiresidue Pesticides in Grapes by PSA-MSPD and GC-MS-SIM

Abstract

The article demonstrates a method of simultaneous determination for 352 pesticide residues in grapes using primary-secondary amine (PSA) matrix solid phase dispersion (MSPD) cleanup and gas chromatography-mass spectrometry-selected ion monitoring (GC-MS-SIM). Grape samples (15 g) were mixed with 6 g of anhydrous magnesium sulfate and 1.5 g of sodium chloride, and then extracted with acetonitrile (15 mL) and cleaned up with 0.3 g of dispersive PSA. The analytes were determined by GC-MS-SIM. Four injections for one sample were acquired to cover a total of 352 pesticides. The limit of detection (LOD) for the method was 0.0017-0.2667 mg kg(-1), depending on the nature of compounds. The linear correlation coefficient (r) was equal to or greater than 0.95; at low, medium, and high fortification levels, recoveries ranged from 45% to 136% for 352 pesticides, among which the recoveries between 60%-120% accounted for 97%. The pesticides for which the relative standard deviations (RSD) were equal to or below 20% accounted for 95%. A positive of nine varieties of grape samples was detected out, one of which was abtained Changli city, Hebei province, China. Pesticides were identified by the retention time, molecule ions, fragment ions, and the abundance ratio of the selected ions. The analytical method was rugged, quick, cheap and effective, and suitable for the determination of a wide scope of 346 pesticides in grapes.

Occurrence and seasonal loads of pesticides in surface water and suspended particulate matter from a wetland of worldwide interest—the Ria Formosa Lagoon, Portugal

“…The target and qualifier ions (MS) were determined by injection of individual pesticide standards, using full-scan mode (40-650 m/z). The product ions were compared with other methods (Lian et al 2010;Rocha et al 2011;Wong et al 2010;X. Yang et al 2011) and supported by NIST Mass Spectral Search Program (version 2.0, 2005) library to create a selected ion monitoring (SIM; Table 1).…”

Distribution and migration study of pesticides between peel and pulp in grape by online gel permeation chromatography–gas chromatography/mass spectrometry

“…High throughput screening methods with simple sample preparation were preferable for target pesticides, such as gas chromatography/mass spectrometry (GC/MS) (Lagunas-Allue, Sanz-Asensio, & Martinez-Soria, 2010;Li, Zhang, & Shi, 2011;Lian et al, 2010;Satpathy, Tyagi, & Gupta, 2011) and liquid chromatography/tandem mass spectrometry (LC-MS/MS) methods (Pico & Kozmutza, 2007;Venkateswarlu, Mohan, Kumar, & Seshaiah, 2007). Furthermore, non-target pesticides should also be considered and timeof-flight (TOF) mass spectrometry (Dasgupta et al, 2010) or the normal GC/MS method with scan mode (Satpathy et al, 2011) was reported for this purpose.…”

Extraction of matrine from soil with matrix solid‐phase dispersion by molecularly imprinted polymers derived from lignin‐based Pickering emulsions

“…At present, this method is mainly used to extract solid, semi‐solid and highly viscous samples . Dispersants used in MSPD are TiO 2 , primary‐secondary amine and so on. However, these dispersants lack selectivity, causing many impurities exist in the eluent.…”