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Multiresidue determination of thermolabile insecticides in cereal products by gas chromatography–mass spectrometry: Evaluation with on‐column injection and conventional hot splitless injection
Author(s) -
Zheng Ping,
Hu YanYun,
Sheng Xuan,
Zhang Lei,
Sun Hao,
Sheng GuoPing
Publication year - 2007
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200700125
Subject(s) - chromatography , chemistry , thermolabile , detection limit , gas chromatography , mass spectrometry , pesticide residue , european union , gas chromatography–mass spectrometry , reproducibility , quechers , pesticide , biochemistry , agronomy , business , biology , enzyme , economic policy
This communication presents a study on the simultaneous determination of thermolabile N ‐methylcarbamate and organophosphorus insecticides in cereal products by gas chromatography–mass spectrometry. The thermal stability of the multiple insecticides was evaluated with conventional hot splitless injection and on‐column injection. The results obtained by GC–MS with these two injection techniques were compared in terms of the recovery, the limit of detection, the limit of qualification, and the reproducibility. With on‐column injection, the pesticide recoveries in cereal samples were better than 82%, with relative standard deviations lower than 5.4%. The limits of qualification for most insecticides were in the range of 0.009–0.08 mg/kg, i. e. lower than the maximum residue limits established for insecticides in cereal products by the European Union. The long‐term stability using on‐column injection for analysis of insecticides in real samples was evaluated and normal chromatographic performance could be obtained within 50 analyses. The results revealed that it was possible for application of on‐column injection in the analysis of thermolabile multiple insecticides in food sample after comprehensive sample clean‐up, despite the highly contaminated nature of the column system.