Method for extraction of dicyandiamide component in dairy product
An extraction method and technology for dairy products, applied in material separation, analytical materials, measuring devices, etc., can solve the problems of detecting and analyzing instrument pollution, reducing instrument sensitivity and service life, etc.
Active Publication Date: 2014-11-05
中华人民共和国温州出入境检验检疫局
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Problems solved by technology
[0005] In order to overcome the deficiencies in the prior art, the present invention provides a method for extracting dicyandiamide in milk products. The method has the advantage of high extraction efficiency, and solves the problem in the prior art because the extracted sample has not undergone effective extraction. Purification means will cause pollution to the detection and analysis instrument, thereby reducing the sensitivity and service life of the instrument
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[0022] Specific embodiments of the present invention are as follows:
[0023] 1. Preparation of instruments and reagents:
[0024] (1) Agilent1200 high performance liquid chromatography (Agilent, USA), API 4000 electrospray tandem mass spectrometer (AB Applied Biosystems, USA); Milli-Q ultrapure water device ((Millipore, USA); ultrasonic cleaner (Elma P300 H, Germany Elma Company), Waters Sep-Pak AC-2 solid-phase extraction column, methanol, acetonitrile are chromatographically pure (German MERCK Company); Formic acid, acetic acid, ammonium acetate (U.S. Alfa Aesar Company); Other reagents are analytical Pure. Experimental milk powder samples were purchased from nearby supermarkets. Dicyandiamide standard products were purchased from China National Institutes for Food and Drug Control, 15 N 4 -marked dicyandiamide standard substance is purchased from Toronto research chemicals Inc (Canada), purity ≥ 99%, (its structure is respectively as figure 1 shown). Use acetonitrile ...
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The invention discloses a method for extraction of a dicyandiamide component in a dairy product. The method comprises preparation of a sample needing to be detected, and purification. Concretely, the method comprises the following steps of adding a formic acid aqueous solution into a dairy product, carrying out microwave extraction to obtain a solution needing to be detected, carrying out centrifugation of the solution needing to be detected, carrying out solid-phase extraction, orderly carrying out water spraying and elution solvent elution to obtain an eluent, carrying out evaporation concentration of the eluent, diluting the eluent by an acetonitrile solvent, and carrying out filtration to obtain a solution of a sample needing to be detected. In a recovery rate test, an internal standard substance is added into a weighed dairy product artificially added with a determined amount of dicyandiamide, the mixture is orderly subjected to the above processes to form a solution of a sample needing to be detected, the solution of the sample is detected by a liquid chromatogram-tandem mass spectrometer so that a dicyandiamide concentration value is determined, and through the detected concentration value and the known concentration value, a recovery rate is calculated and is in a range of 83.6-95.7%. The method has the advantages of high extraction efficiency and good reappearance.
Description
technical field [0001] The invention relates to a method for extracting dicyandiamide, in particular to a method for extracting dicyandiamide in dairy products. Background technique [0002] Dicyandiamide, also known as dicyandiamide, dicyandiamide, abbreviated as DICY or DCD, is a white crystalline powder. in the water Solubility It is 2.26% at 13°C, and has a relatively high solubility in hot water. When the aqueous solution is gradually decomposed at 80°C, it will produce Ammonia . Low toxicity, median lethal dose (mice, oral)>4000mg / kg. The maximum allowable concentration in the air is 5mg / m 3 . It is mainly used as raw material of melamine, dye fixing agent, chemical fertilizer, fine chemical intermediate, etc. At present, international standards do not limit dicyandiamide in food, but high doses of dicyandiamide are toxic to the human body. Milk products containing dicyandiamide may have side effects on infants and young children. The functions are not per...
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IPC IPC(8): G01N30/08G01N30/14
Inventor 韩超刘翠平陈祥准刘滨朱振瓯
Owner 中华人民共和国温州出入境检验检疫局