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    Home > Chemicals Industry > Chemical Technology > Determination of 18 sulfonamide residues in royal jelly by liquid chromatography-tandem mass spectrometry (1)

    Determination of 18 sulfonamide residues in royal jelly by liquid chromatography-tandem mass spectrometry (1)

    • Last Update: 2021-09-04
    • Source: Internet
    • Author: User
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    2.
    1 Scope of application

    Suitable for 18 kinds of sulfonamides in royal jelly ( sulfadiazine , sulfathiazole , sulfapyridine, sulfamethazine, sulfamethoxine , sulfamethizole, sulfamethazine, sulfamethoxazole , sulfamethoxazole) Pyrimidine, Sulfachloropyridazine, Sulfamethoxazole, Sulfamethoxazole, Sulfamethoxazole, Sulfamethoxazole, Sulfachloropyrazine, Sulfapyrazole, Sulfamethoxazole Quinoxaline) residual liquid chromatography
    .


    Zhonglian mass spectrometry


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    2 Principle of the method

    The residues of sulfonamides in royal jelly were extracted with deionized water, and the protein was precipitated with trichloroacetic acid .
    After centrifugation, the supernatant was purified by Oasis MCX ion exchange column or equivalent solid phase extraction column, and ammonia-methanol solution (1+19, v /v) After elution and drying, the residue is dissolved with acetonitrile-0.
    01mo/L ammonium acetate solution, and after passing through a 0.
    2um filter membrane, the sample solution is measured by liquid chromatography-tandem mass spectrometer and quantified by internal standard method
    .

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    3 Reagents and materials

    Methanol, acetonitrile: chromatographic purity: ammonium acetate, trichloroacetic acid, formic acid, ammonia water: analytically pure; 0.
    01mol/L ammonium acetate solution; weigh 0.
    77g ammonium acetate and dissolve in 1000mL water; 2% formic acid solution: draw 2mL formic acid and dilute with water To 100mL: 50% trichloroacetic acid solution: Weigh 20g of trichloroacetic acid dissolved in 20mL of water ammonia-methanol solution: (1+19, v/v), suck 5mL ammonia and 95mL methanol and mix well; Acetonitrile -0.
    01mo/L Ammonium acetate solution (3+22, v/v): Measure 12mL acetonitrile and 88mL ammonium acetate solution and mix well
    .


    18 kinds of sulfa standard materials: purity>99%


    0.
    1 mg/mL standard stock solution: accurately weigh an appropriate amount of each sulfonamide standard substance, and use methanol to prepare a 0.
    1 mg/mL standard stock solution.
    The solution is stored at 4°C
    .

    5.
    0ug/mL sulfonamide mixed standard working solution: Pipette 0.
    5mL of each standard stock solution into a 10mL volumetric flask, and dilute with methanol to a 5.
    0ug/mL mixed standard working solution
    .


    The solution is stored at 4°C


    Sulfa internal standard substances: sulfamethoxazole-D4, sulfadiazine-D4, sulfathiazole-D4
    .


    Purity ≥99%


    0.
    1mg/mL sulfamethoxazole-D4, sulfadiazine-D4, sulfaoxazole-D4 internal standard stock solution: Weigh appropriate amount of sulfamethoxazole-D4, sulfadiazine-D4, sulfathiazole-D4 standards Substances were made up to 0.
    1mg/mL with methanol
    .


    The solution is stored at 4°C


    Mixed internal standard working solution: Pipette 0.
    5 mL each of the sulfamethoxazole-D4, sulfadiazine-D4, and sulfadioxazole-D4 stock solutions into a 10 mL volumetric flask, dilute to the mark with methanol, and keep the solution at 4°C Save
    .

    Matrix standard working solution: draw different volumes of standard working solution and 20μL mixed internal standard working solution, and use blank sample extract to make 5.
    0ng/mL, 10.
    0ng/mL, 20.
    0ng/mL, 50.
    0ng/mL, 100.
    0ng/mL Different concentrations of matrix standard working solutions
    .


    Prepared on the same day


    Oasis MCX column or equivalent: 150mg, 6mL
    .


    Treat with 5mL methanol and 10mL water in sequence before use


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    4 Apparatus and equipment

    Liquid chromatography-tandem mass spectrometer: equipped with electrospray ion source: analytical balance: sensitivity 0.
    1mg and 0.
    01g; polypropylene test tube with stopper: 50mL; oscillator, liquid mixer; solid phase extraction device: glass storage Liquid container: 50mL; nitrogen concentrator; concentration tube: 10mL
    .

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    5 Sample pretreatment

    (1) Each sample system

    (2) Extraction

    Weigh 2g sample, accurate to 0.
    01g
    .


    Place it in a 50mL polypropylene test tube with a stopper, add 20uL of internal standard working solution, then add 20mL of water, mix quickly on a liquid mixer for 1 min, then place on a shaker to shake and extract for 10 min, add 0.


    (3) Purification

    For frozen laboratory samples, stir them evenly after thawing
    .
    Separate 0.
    5 kg as a sample
    .
    The prepared sample is placed in a sample bottle, sealed, and marked
    .
    The samples were frozen and stored at -18°C
    .

    Connect the glass reservoir plugged with glass wool to the Oasis MCX column, pour the supernatant into the glass reservoir, adjust the flow rate to less than 3mL/min, and wait for the sample solution to flow out completely, use 5mL formic acid solution and 5mL in turn Wash the column with methanol and discard all the effluent
    .
    Finally, it was eluted with 5 mL ammonia-methanol solution, and the eluate was collected in a 10 mL concentrating tube
    .
    Blow dry at 50°C with a nitrogen concentrator
    .
    Accurately add 1.
    0mL acetonitrile-0.
    01mo/L ammonium acetate solution to dissolve the residue.
    After the sample solution is passed through a 0.
    2um filter membrane, it is used for liquid chromatography-tandem mass spectrometer determination
    .

    According to the above extraction and purification steps, a blank sample extract solution for preparing a series of matrix standard working solutions is prepared
    .

     

     

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