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    Home > Chemicals Industry > Chemical Technology > Scope of application and method principles for determination of residues of streptomycin, dihydrostreptomycin and kanamycin in milk powder, milk, puffer fish, eel and royal jelly

    Scope of application and method principles for determination of residues of streptomycin, dihydrostreptomycin and kanamycin in milk powder, milk, puffer fish, eel and royal jelly

    • Last Update: 2021-11-05
    • Source: Internet
    • Author: User
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    3.
    2.
    1.
    1 Scope of application

    It is suitable for the determination of residues of streptomycin , dihydrostreptomycin and kanamycin in milk powder, milk, puffer fish, eel and royal jelly
    .


    The detection limit of the method: milk, puffer fish, eel, and royal jelly are all 10.


    3.
    2.
    1.
    2 Principle of the method

    The antibiotic in the sample is extracted with phosphoric acid solution, and the protein is precipitated with trichloroacetic acid , and purified with benzene sulfonic acid type and carboxylic acid type solid phase extraction column
    .


    Detected by liquid chromatography-tandem mass spectrometer (ESI+) and quantified by external standard method


    3.
    2.
    1.
    3 Reagents and materials

    Methanol, acetonitrile: chromatographically pure
    .


    Formic acid, concentrated phosphoric acid, dipotassium hydrogen phosphate (K 2 HPO 4 ), trichloroacetic acid (C 2 HC1 3 O 2 ), sodium heptane sulfonate (C 4 H 15 NaO 3 ·SH 2 O): pure superior grade


    5% phosphoric acid solution (1+19, v/v): Take 50mL concentrated phosphoric acid and dilute to 1L with water
    .

    0.
    2mol/L phosphate buffer solution: pH=8.
    5
    .


    Weigh 34.


    Trichloroacetic acid solution: 50%, mass fraction
    .


    Take 20g of trichloroacetic acid and dilute to 20mL with water

    0.
    01mol/L sodium heptane sulfonate solution: Weigh 2.
    20 g sodium heptane sulfonate, dissolve in water, and dilute to 1L
    .

    SPE elution solution: Take 4 mL of formic acid and dilute to 100 mL with 0.
    01 mol/L heptane sulfonate solution
    .

    25% methanol solution (1+3, v/v): Take 25 mL of methanol and dilute to 100 mL with water
    .

    Standard material: all purity >98%
    .

    1.
    0mg/mL standard stock solution: Weigh appropriate amounts of streptomycin, dihydrostreptomycin and kanamycin standard substances, respectively dissolve them with 0.
    3% acetic acid aqueous solution and prepare 1.
    0mg/mL standard stock solutions
    .


    Store in a freezer at -18°C protected from light


    0.
    1ug/mL mixed standard solution: draw an appropriate amount of streptomycin, dihydrostreptomycin and kanamycin standard stock solution, dilute with 0.
    3% acetic acid water to a 0.
    1ug/mL mixed standard solution
    .


    Store in a freezer at -18°C protected from light


    Benzenesulfonic acid type solid phase extraction column (500mg, 3mL) or equivalent
    .


    Before use, pretreated with 5mL methanol and 10mL water successively to keep the column moist


    Carboxylic acid type solid phase extraction column (500mg, 3mL) or equivalent
    .


    Before use, pretreated with 5mL methanol and 10mL water successively to keep the column moist
    .

    Filter membrane: 0.
    2um
    .

    3.
    2.
    1.
    4 Instruments and equipment

    Liquid chromatography-tandem quadrupole mass spectrometer, equipped with electrospray ion source
    .
    Analytical balance: Sensitivity 0.
    1mg and 0.
    01g
    .
    Liquid mixer
    .
    Solid phase extraction device
    .
    Oscillator
    .
    Vacuum pump: the vacuum degree should reach 80kPa
    .
    Micro syringe: 25μL, 100uL
    .
    pH meter: measurement accuracy ±0.
    02pH unit
    .
    Centrifuge tube with stopper: 100mL
    .
    Graduated centrifuge tube: 5mL
    .
    Reservoir: 50mL
    .
    Centrifuge: The speed is above 4000r/min
    .

    Related links: Determination of residues of aminoglycoside drugs (5)

     

     

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