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    Home > Chemicals Industry > Chemical Technology > Liquid chromatography-tandem mass spectrometry for the determination of melengestrol acetate, chlorgestrol acetate and megestrol acetate residues in milk and milk powder

    Liquid chromatography-tandem mass spectrometry for the determination of melengestrol acetate, chlorgestrol acetate and megestrol acetate residues in milk and milk powder

    • Last Update: 2021-09-12
    • Source: Internet
    • Author: User
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    8.
    2.
    2.
    1 Scope of application

    It is suitable for the determination of melengestrol acetate , chlorgestrol acetate and megestrol acetate residues in milk and milk powder by liquid chromatography tandem mass spectrometry
    .


    The detection limit of the method: the detection limit of melengestrol acetate, megestrol acetate and chlorgestrol acetate in milk are all 2μg/kg; the detection limit of melengestrol acetate, megestrol acetate and chlorgestrol acetate in milk powder are all 2μg/kg; The detection limit of ketone is 20μg/kg


    8.
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    2 Principle of the method

    After the fat is extracted from the milk sample, it is extracted with acetonitrile , and after saponification, it is purified by a cyanopropyl solid phase extraction column, separated by a C 18 chromatographic column, detected by liquid chromatography-tandem mass spectrometry, and quantified by an external standard method
    .

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    3 Reagents and materials

    Acetonitrile, methanol, ethyl acetate , n-hexane: chromatographically pure; magnesium chloride (MgCl 2 : 6H 2 O), sodium hydroxide , formic acid, 25% ammonia, 95% ethanol, petroleum ether , anhydrous sodium sulfate : analytically pure
    .

    Ethyl acetate + n-hexane (1+19, v/v): Measure 10 mL of ethyl acetate and mix with 190 mL of n-hexane
    .


    Ethyl acetate + n-hexane (1+4, v/v): measure 40 mL of ethyl acetate and mix with 160 mL of n-hexane


    Acetonitrile + water (7+3, v/v): Measure 700 mL of acetonitrile and mix with 300 mL of water, and shake well
    .

    Standard materials: melengestrol acetate, chlorgestrol acetate and megestrol acetate, with purity ≥97%
    .

    1000μg/mL standard stock solution: accurately weigh out 0.
    0500g of melengestrol acetate, chlorgestrol acetate and megestrol acetate standard substances in a 50mL volumetric flask, dissolve it with methanol and make the volume constant
    .


    The standard stock solution is stored at 4°C


    100μg / mL standard solution mixing the I
    .


    Draw 10.


    1.
    0ug/mL mixed standard solution II
    .


    Take 1.


    Matrix mixed standard working solution: Take an appropriate amount of mixed standard solution II, and use the blank sample extract to prepare matrix mixed standard solutions of different concentrations
    .


    The standard working solution is ready to use


    Cyanopropyl solid phase extraction column or equivalent: 3mL/500mg
    .


    Before use, rinse with 5mL ethyl acetate and 6mL n-hexane respectively to keep the column moist


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    4 Instruments and equipment

    Liquid chromatography-tandem mass spectrometer: equipped with electrospray ionization source (ESI)
    .


    Analytical balance: Sensitivity 0.


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