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Ultra-trace determination of sodium fluoroacetate (1080) as monofluoroacetate in milk and milk powder by GC-MS/MS and LC-MS/MS

Abstract

A sensitive analytical method based on derivatization with 3-nitroaniline is established for the trace determination of sodium fluoroacetate (1080) in milk and milk powders. The method reported here utilizes protein precipitation by tungstic acid, solid phase extraction (SPE) clean-up in pass-through mode with mixed-mode anionic exchange (MAX) cartridge and N,N’-dicyclohexylcarbodiimide (DCC) mediated derivatization with 3-nitroaniline (3-NA). The derivative 2-fluoro-N-(3-nitrophenyl)acetamide (MFA-3NA) can be determined with both gas chromatography tandem mass spectrometry (GC-MS/MS) and liquid chromatography tandem mass spectrometry (LC-MS/MS). In our study, negative chemical ionization (NCI) gas chromatography tandem massspectrometry (GC-MS/MS) and electrospray ionization (ESI) liquid chromatography tandem mass spectrometry (LC-MS/MS) in negative ionization mode were used. Quantification of the MFA-3NA was accomplished by using matrix-matched calibration with stable isotope labeled sodium monofluoroacetate (13C2D2-MFA) as internal standard (I.S.). The method was validated with MFA fortified milk samples at 0.1, 0.2 and 0.4 µg/L and milk powder samples at 0.5, 1 and 2 µg/kg. In GC-MS/MS, the LOQs in milk and milk powder samples were 0.0042 µg/L and 0.0085 µg/kg, respectively. The RSDs at all spike levels for milk and milk powder samples were less than 6% with recoveries ranging from 90 to 105%. In LC-MS/MS, the LOQs in milk and milk powder samples were 0.00033 µg/L and 0.0088 µg/kg, respectively. The RSDs at all spike levels for milk and milk powder samples were less than 13% with recoveries ranging from 90 to 112%. The proposed method has been applied to detect 1080 as monofluoroacetate (MFA) in milk and milk powder samples purchased from the local market.

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Publication details

The article was received on 06 Apr 2018, accepted on 09 Jun 2018 and first published on 11 Jun 2018


Article type: Paper
DOI: 10.1039/C8AY00767E
Citation: Anal. Methods, 2018, Accepted Manuscript
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    Ultra-trace determination of sodium fluoroacetate (1080) as monofluoroacetate in milk and milk powder by GC-MS/MS and LC-MS/MS

    Y. Wong, W. Law, S. S. Lai, S. Wong, K. Lau and C. Ho, Anal. Methods, 2018, Accepted Manuscript , DOI: 10.1039/C8AY00767E

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