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    Home > Chemicals Industry > Chemical Technology > Determination of Estradiol Residues in Aquatic Products - Gas Chromatography-Mass Spectrometry (1)

    Determination of Estradiol Residues in Aquatic Products - Gas Chromatography-Mass Spectrometry (1)

    • Last Update: 2022-08-19
    • Source: Internet
    • Author: User
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    1 Scope

    This standard specifies the method for the determination of β-estradiol residues in aquatic products by gas chromatography-mass spectrometr.


    This standard applies to the determination of β-estradiol residues in edible parts of aquatic product.


    beta-estradiol

    2 Normative references

    The clauses in the following documents become clauses of this standard through reference in this standar.


    GB/T 6682 Analysis Laboratory Water Specifications and Test Methods

    3 Principles

    Under acidic conditions, β-estradiol in the sample was extracted with acetonitrile, degreased with n-hexane, purified with C18 solid phase extraction column, derivatized with silanization reagent, and then determined by gas chromatography-mass spectrometer, and quantified by internal standard metho.


    n-hexane

    4 Reagents

    1 All reagents should have no interference peak.


    2 β-estradiol standard: purity ≥97.


    3 β-estradiol-D2 standard: purity ≥98.


    4 Acetonitrile: chromatographically pur.


    5 Methanol: chromatographically pur.


    6 n-hexane: chromatographically pur.


    7 n-Propano.


    8 Sodium acetate buffer solution (2mol/L, pH2): Take 237mL of 2mol/L sodium acetate solution and 63mL of 2mol/L acetic acid solution, mix well, and adjust to pH2 with glacial acetic aci.


    9 Acetic acid solution (1%): take 25mL of glacial acetic acid, dissolve in water, and dilute to 250m.


    10 β-estradiol standard stock solution: Accurately weigh 01 g of β-estradiol, dissolve it in methanol, and dilute it to a 100 mL volumetric flask to make a standard solution with a concentration of 100 μg/mL, and store it at -18°.


    11 β-estradiol internal standard stock solution: Accurately weigh 01 g of β-estradiol-D2, dissolve in methanol, and dilute to a 50 mL volumetric flask to make a standard solution with a concentration of 200 μg/mL, at -18° C storage, the storage time does not exceed 6 month.


    12 β-estradiol standard working solution: before use, accurately draw the β-estradiol standard stock solution, dilute it with methanol to a concentration of 005μg/mL~25μg/mL standard working solution, and temporarily store it at 4°.


    13 β-estradiol-D2 internal standard working solution: Before use, accurately draw the internal standard standard stock solution, dilute it with methanol to a standard working solution with a concentration of 05 μg/mL, and temporarily store it at 4°.

    14 Derivatization reagent: accurately weigh 01g dithioerythritol (DTE), dissolve it in 5mL N-methyltrimethylsilyl trifluoroacetamide (MSTFA), and then add 10μL trimethyl Iodosilane (TMIS), mixed well, placed at 4°C overnight before use, and stored in a sealed container away from light and moistur.
    The derivatization reagent should be colorless, if there is a color change such as brown-red, it indicates that the reagent is invali.

    Erythritol

    5 Instruments

    1 Gas chromatography single quadrupole mass spectrometer: equipped with electron impact ionization (EI) ion sourc.

    2 Electronic balance: Sensitivity 0001.

    3 Vortex mixe.

    4 High-speed refrigerated centrifuge: the maximum speed is 10 000r/mi.

    5 Solid phase extraction apparatu.

    6 Nitrogen blowe.

    7 Centrifuge tube with stopper: 50m.

    8 Chicken heart bottle: 50m.

    9 Glass tube with stopper scale: 10m.

    10 C18 solid phase extraction column: packing 500mg/3mL, choose Cleanert ODSC18 (end-capped), or equivalen.

    11 Sample reaction vial: 2mL, deactivated, threade.

     

     

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