Multiresidue Analysis of Pesticides in Animal and Fishery Products by NCI mode GC/MS and Dual-column GC-micro ECD

Abstract

A sensitive and quantitative multiresidue method using NCI mode GC/MS and GC-micro ECD for determining pesticides in animal and fishery products was established. The crude sample extract obtained by acetoneῌhexane extraction for solid samples or acetonitrile extraction for liquid samples was cleaned up with a GPC/SPE system. The first GPC pesticide fraction containing lipids and pigments was selectively collected, and loaded directly onto a graphitized carbon/PSA 2-layered column. After the second GPC pesticide fraction was collected, the 2-layered column was eluted with acetoneῌhexane (3 : 7). The combined eluate was subjected to NCI-SIM/Scan mode GC/MS for semi-quantification. After fractionation by Florisil cartridge column SPE, each fraction was subjected to dual-column GC-micro ECD for quantification. Average recoveries (n̮5) of pesticides, except for chlorothalonil and some others, from fortified samples ranged from 76.8̮ to 107.9̮ with RSD values of ̮9.7̮. (Received May 26, 2008)Key words: Q̲̰Ὸ pesticide residue; ῖQQ΅ animal and fishery product; ῴQῢ̱ ̲Ό̱ ̲ῼῲῐ gel permeation chromatography (GPC); QῐῘQ solid-phase extraction (SPE); ῬQ Qῳ̱ Q negative chemical ionization (NCI); ̱ῶ̱ ̲Ό̱̲ῼῲῐ gas chromatography (GC); Q̲`Q̱ mass spectrometry (MS); ̲ῳ̱ ̯Q̱QQQQQ micro-electron capture detector (micro ECD)

Validation of multi-residue method for determination of pesticides in meat products using official guideline of analytical methods in Japan

“…2) In addition, some pesticides were difficult to detect because of interfering compounds from meat products; therefore, we improved the official method and developed a multi-residue screening method for meat products using GC-MS and LC-MS. 3) Many pesticides with a wide range of polarity were successfully extracted with ethyl acetate-cyclohexane (1 : 1), instead of acetone-nhexane (1 : 2) used in the official method. The interfering compounds were effectively eliminated by means of gel permeation chromatography (GPC), and primary secondary amine (PSA) and silica-gel mini-column solid-phase extraction (SPE).…”

Development and diffusion of a systematic method for determination of multiple pesticide residues in agricultural products

“…ESI electrospray ionization -Scheduled MRM LC-MS/MS 31,34,35 MS/MS 1 EI-SIM/Scan GC-MS 13 NCI negative chemical ionization -SIM/Scan GC-MS 23 GC-ECD/ECD 7,15,16 FPD ame photometric detector NPD nitrogen phosphorus detector GC-FPD/NPD 8 10,16 PDA photodiode-array detector ESI-SIM/Scan LC-PDA/MS 17,19 N- solid-phase extraction, SPE 7 12 gel permeation chromatography, GPC GPC -Nprimary secondary amine, PSA GPC-SPE Fig. 4 13, 17,23 GC-MS /MS Fig. 3.…”