Multiresidue method to quantify pesticides in fish muscle by QuEChERS-based extraction and LC-MS/MS

Abstract

Pesticide residues in fish muscle are an environmental and a health safety concern which requires analytical methods presenting high sensitivity and low limits of quantification. In this study, adapted QuEChERS method, coupled to liquid chromatography tandem mass spectrometry (Scheduled MRM-5500 QTRAP), was developed to quantify 13 pesticides (azoxystrobin, clomazone, diflufenican, dimethachlor, carbendazim, iprodion, isoproturon, mesosulfuron-methyl, metazachlor, napropamid, quizalofop and thifensulfuron-methyl) in muscle of fish. Quantification limits were below 1 ng g(-1) except for clomazone (1.8 ng g(-1)) and quizalofop (7.4 ng g(-1)). Best recoveries were observed for perch (>80%) and roach (>68%), except for thifensulfuron-methyl. Lower recoveries had been observed for carp (6% to 86%). Relative standard deviation was lower than 28% for intra-day and 29% for inter-day analysis, respectively. This method was successfully tested on three fish species, naturally or orally exposed: roach (Rutilus rutilus), perch (Perca fluviatilis) and carp (Cyprinus carpio). Few levels were observed in fish naturally exposed, but carp and perch orally contaminated showed measurable levels in their muscles.

Liquid Chromatography-Mass Spectrometry in the Analysis of Pesticide Residues in Food

“…In the analysis of pesticide residues in food, the quadrupole-linear ion trap tandem mass spectrometer has been used mainly to analyze pesticide residues in vegetables and fruit (Sinha et al 2012;Afify et al 2010;Lee et al 2009a, b;Pihlstrom et al 2007;Banerjee et al 2007), (Lee et al 2009a, b), cocoa beans (Zainudin et al 2015), lavandin oil (Fillatre et al 2014) fruit beverages (Tran et al 2012;Ferrer et al 2011), and fish muscle (Lazartigues et al 2011). …”

Next Generation Instruments and Methods for Proteomics

“…Several authors have reported good results after using this high-sensitive instrument, allowing the simultaneous identification and quantification of the proteins of interest (Grobosch et al, 2012;Janeckova et al, 2012;Lazartigues et al, 2011;Li et al, 2011;Paine et al, 2012;Rust et al, 2012;Wu et al, 2011).…”

Study of matrix‐induced effects in multi‐residue determination of pesticides by online gel permeation chromatography‐gas chromatography/mass spectrometry

“…Enhancement effects were found for most of the carbamate pesticides in matrix (Nos. 3,7,9,11,14,18,21,22,25,27,33,42,60, 65, 69, 108, 136, Table 3). The repetitions were also good (RSDs below 15%) and the online GPC-GC/MS method was suitable to measure these pesticides if calibrated by matrix-matched standards.…”

“…Extensive sample preparation methods were reported to remove interference before measurement, such as solid-phase extraction (SPE), [2,[4][5][6][7] gel permeation chromatography (GPC) [5,[8][9][10][11] and the quick, easy, cheap, effective, rugged and safe sample preparation method (QuEChERS protocol, a method derived from the dispersive SPE with the use of primary secondary amine (PSA) as sorbent). [5,[12][13][14][15][16][17] Buffering QuEChERS methods were developed to improve the recoveries of pH-dependent pesticides. [18][19][20][21][22][23] Analyte protectants were applied to block the active sites in the instruments.…”