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    Home > Chemicals Industry > Chemical Technology > Determination of 9 Penicillin Residues in Livestock and Poultry Meat——Applicable Scope and Method Principle

    Determination of 9 Penicillin Residues in Livestock and Poultry Meat——Applicable Scope and Method Principle

    • Last Update: 2021-09-20
    • Source: Internet
    • Author: User
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    5.
    2.
    1.
    1 Scope of application

    It is suitable for the determination of 9 penicillin residues in cattle, sheep, pigs and chicken by liquid chromatography-tandem mass spectrometry
    .


    Detection limit of the method: Nafcillin is 0.


    5.
    2.
    1.
    2 Principle of the method

    9 kinds of penicillin residues in the sample, extracted with 0.
    15mol/L sodium dihydrogen phosphate (pH8.
    5) buffer solution, centrifuged, the supernatant was purified with a solid phase extraction column, determined by liquid chromatography-tandem mass spectrometry, external standard Method quantitative
    .

    5.
    2.
    1.
    3 Reagents and materials

    Both methanol and acetonitrile are chromatographically pure; sodium dihydrogen phosphate (NaH 2 PO 4 ), sodium hydroxide , and acetic acid are all top grade pure; acetonitrile + water (1+1, v/v): measure 50 mL acetonitrile and 50 mL water Mix; Sodium hydroxide solution: 5mol/L
    .


    Weigh 20g of sodium hydroxide, dissolve in water, and dilute to 100mL; sodium dihydrogen phosphate buffer solution: 0.


    Amoxicillin, ampicillin, piperacillin, penicillin G, penicillin V, oxacillin, cloxacillin, nafcillin, and dicloxacillin 9 standard penicillin standards: purity ≥99%
    .

    Nine penicillin standard stock solutions: accurately weigh an appropriate amount of each standard substance, and prepare a standard stock solution with a concentration of 1.
    0 mg/mL with water
    .


    The stock solution is stored in a -18°C freezer


    9 kinds of penicillin standard working solutions: draw an appropriate amount of each penicillin standard stock solution as needed, and dilute with the blank sample extract to form a matrix mixed standard working solution of appropriate concentration
    .

    BUNDELUT C18 solid phase extraction column or equivalent: 500mg, 6mL
    .


    Before use, pretreated with 5mL methanol, 5mL water and 10mL sodium dihydrogen phosphate buffer solution to keep the column moist


    5.
    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; oscillator; solid phase extraction vacuum device; reservoir: 50mL; micro syringe: 25μL, 100μL ; Scaled sample tube: 5mL, with an accuracy of 0.
    1mL; centrifuge: with a 50mL centrifuge tube with stopper; pH meter: measurement accuracy of 0.
    02pH unit
    .

    5.
    2.
    1.
    5 Sample pretreatment

    Weigh 3g sample (accurate to 0.
    01g) into a 50mL centrifuge tube, add 25mL sodium dihydrogen phosphate buffer solution, shake on a shaker for 10 minutes, then centrifuge at 4000r/min for 10 minutes, and move the upper extract to the bottom In the reservoir connected to the BUNDELUT C 18 solid phase extraction column, pass through the solid phase extraction column at a flow rate of 3 mL/min, wash the column with 2 mL of water, and discard all the effluent
    .


    Elute with 3mL of acetonitrile+water, collect the eluate in a graduated sample tube, dilute to 3mL with acetonitrile+water, shake well, pass through a 0.


     

     

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