Chinese Journal of Chromatography

Chinese Journal of Chromatography ›› 2015, Vol. 33 ›› Issue (11): 1175-1185.DOI: 10.3724/SP.J.1123.2015.07012

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Determination of 213 pesticide residues in milk and milk power by gas chromatography-triple quadrupole tandem mass spectrometry

WANG Jing1, AI Lianfeng1, MA Yusong1, ZHANG Haichao1, LI Wei1, YU Meng2   

  1. 1. Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang 050051, China;
    2. College of Food Science and Technology, Agricultural University of Hebei, Baoding 071000, China
  • Received:2015-07-10 Online:2015-11-08 Published:2012-05-30

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Abstract:

On the basis of the optimization of solid phase extraction adsorbent, eluting solvent types and amounts, a gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS) method was established for the determination of 213 pesticide residues in milk and milk power. The samples were extracted by acetonitrile, cleaned-up with an ENVI-Carb/NH2 solid-phase extractant, and determined by GC-MS/MS using external standard method. The linear ranges were from 10 to 1000 μ g/L for 197 pesticides, from 50 to 1000 μ g/L for the other 16 pesticides with the correlation coefficients higher than 0.99. The limits of detection (LODs, S/N=3) varied over the range of 0.03 to 7.59 μ g/kg, and limits of quantification (LOQs, S/N=10) ranged from 0.10 to 21.94 μ g/kg. The average recoveries in different matrices were in the range of 66.9%-120.1% with the relative standard deviations (RSDs) of 1.23%-17.6%. This method is simple, rapid, sensitive and reliable for meeting the requirements for the simultaneous identification and quantification of the multi-residues in milk and milk power.

Key words: gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS), milk, milk power, pesticide residues

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