Determination of acephate and methamidophos in tissues: appearance of matrix effect in gas chromatography–mass spectrometry

Springer Science and Business Media LLC - Tập 29 - Trang 159-162 - 2011
Nobuyuki Adachi1,2, Hiroshi Kinoshita3, Minori Nishiguchi1, Motonori Takahashi1, Harumi Ouchi1, Takako Minami1, Kiyoshi Matsui1, Takehiko Yamamura1, Shie Yoshida1, Hajime Nishio1
1Department of Legal Medicine, Hyogo College of Medicine, Nishinomiya, Japan
2Joint-Use Research Facilities, Hyogo College of Medicine, Hyogo, Japan
3Department of Forensic Medicine, Faculty of Medicine, Kagawa University, Kagawa, Japan

Tóm tắt

A simple and reliable method to determine acephate and methamidophos in mammalian tissues is presented. The method includes solid-phase extraction of tissue extracts with active carbon cartridges followed by gas chromatography–mass spectrometry analysis. During the study, a matrix effect was observed especially at low concentrations of acephate and methamidophos in serum and in brain. To minimize the effect, we prepared calibration curves with relatively short ranges. The validation data, such as the linearity of calibration curves, limits of detection, and coefficients of variation for recovery rates, were generally satisfactory. The present method is useful for determination of acephate and methamidophos in mammalian tissues because of its simplicity and speed, keeping in mind the presence of the matrix effect.

Tài liệu tham khảo

Tomlin CDS (ed) (1997) The pesticide manual, 11th edn. British Crop Protection Council, Surrey, pp 7–8, 808–809 Inoue S, Saito T, Miyazawa T, Mase H, Inokuchi S (2009) A simple method for detecting fenitrothion, its metabolite 3-methyl-4-nitrophenol, and other organophosphorus pesticides in human urine by LC-MS. Forensic Toxicol 27:32–36 Kudo K, Ishida T, Hikiji W, Usumoto Y, Umehara T, Nagamatsu K, Tsuji A, Ikeda N (2010) Pattern of poisoning in Japan: selection of drugs and poisons for systematic toxicological analysis. Forensic Toxicol 28:25–32 Adachi N, Kinoshita H, Nishiguchi M, Takahashi M, Ouchi H, Minami T, Matsui K, Yamamura T, Ohtsu N, Yoshida S, Hishida S (2008) Simultaneous analysis of acephate and methamidophos in human serum by improved extraction and GC–MS. Forensic Toxicol 26:76–79 Russo MV, Campanella L, Avino P (2002) Determination of organophosphorus pesticide residues in human tissues by capillary gas chromatography–negative chemical ionization mass spectrometry analysis. J Chromatogr B 780:431–441 Niessen WMA, Manini P, Andreoli R (2006) Matrix effects in quantitative pesticide analysis using liquid chromatography–mass spectrometry. Mass Spectrom Rev 25:881–899 Kruve A, Künnapas A, Herodes K, Leito I (2008) Matrix effects in pesticide multi-residue analysis by liquid chromatography–mass spectrometry. J Chromatogr A 1187:58–66 Ismaiel OA, Zhang T, Jenkins RG, Karnes HT (2010) Investigation of endogenous blood plasma phospholipids, cholesterol and glycerides that contribute to matrix effects in bioanalysis by liquid chromatography/mass spectrometry. J Chromatogr B 878:3303–3316 Albero B, Sánchez-Brunete C, Tadeo JL (2005) Multiresidue determination of pesticides in juice by solid-phase extraction and gas chromatography–mass spectrometry. Talanta 66:917–924 Sánchez-Brunete C, Albero B, Martín G, Tadeo JL (2005) Determination of pesticide residues by GC–MS using analyte protectants to counteract the matrix effect. Anal Sci 21:1291–1296