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    Home > Chemicals Industry > Chemical Technology > Selection of analysis conditions for 8 kinds of macrolides and lincosamide residues in puffer fish and eels

    Selection of analysis conditions for 8 kinds of macrolides and lincosamide residues in puffer fish and eels

    • Last Update: 2021-09-20
    • Source: Internet
    • Author: User
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    6.
    2.
    4.
    7 Selection of analysis conditions

    (1) Selection of extraction solution

    This method compares the main extraction solutions for extracting macrolide drugs from animal tissues, including phosphate buffer solution, 0.
    3% metaphosphoric acid - methanol solution, acetonitrile , Tris solution and acetate solution.
    The experimental results are shown in Table 6.
    -30
    .

    Table 6-30 The extraction effect of different extraction solutions (puffer fish, 50μg/kg, %)

    From the data in Table 6-30, it can be seen that when 0.
    1 mol/L phosphate buffer solution is used as the extracting solution, the recovery rate of 8 kinds of macrolide antibiotics is unreliable; when 0.
    3% metaphosphoric acid methanol solution ( 7+3) When used as an extract, the recovery rate of lincomycin is less than 70%, the recovery rate of erythromycin is very unstable (30%~106%), and the recovery rate of the other 6 macrolide antibiotics More than 70%; when acetonitrile is used as the extracting solution, the recovery rates of 6 kinds of macrolide antibiotics are less than 31.
    4% , except for elixiromycin and tylosin , which are greater than 70%; when using 0.
    1 When the mol/L acetate solution is used as the extract, the recovery rate of spiramycin is 154.
    0%, the recovery rate of tilmicosin is less than 70%, and the recovery rates of the other 6 macrolide antibiotics are all greater than 70%; When Tris solution is used as the extracting solution, the recovery rate of 8 kinds of macrolide antibiotics is in the range of 78.
    4%-99.
    1%
    .


    Therefore, this method uses Tris solution as the extraction solution


    (2) The influence of different solid phase extraction columns on the recovery rate

    Under the aforementioned selected conditions, the extraction efficiency of Varian C 18 , OasisHLB (500), OasisHLB (200), MCX and Bakerbondspe C 18 solid phase extraction columns were compared.
    The results are shown in Table 6-31
    .


    The results show that the OasisHLB(500) solid phase extraction column has the best effect


    Table 6-31 The influence of different solid phase extraction columns on the recovery rate (puffer fish, 50μg/kg, %)

    (3) Selection of internal standard

    Roxithromycin and lincomycin are the main internal standards for the determination of macrolides .
    The comparative experimental results are shown in Table 6-32
    .

    Table 6-32 Selection of different internal standards (pufferfish, 50μg/kg, %)

    From the data in Table 6-32, it can be seen that when lincomycin is used as the internal standard, only the three macrolide antibiotics of Tilmicosin, Kitasamycin and Josamycin have a recovery rate of 94.
    2 %~96.
    5%; when Roxithromycin is used as the internal standard, the recovery rate of 8 kinds of macrolide antibiotics is in the range of 76.
    5%~117.
    0%
    .


    Therefore, this method uses roxithromycin as the internal standard


    6.
    2.
    4.
    8 Linearity range and lower limit of determination

    Prepare a series of matrix standard mixed working solutions with four concentration levels of 2.
    0ng/mL, 4.
    0ng/mL, 10.
    0ng/mL, and 50.
    0ng/mL, and measure under selected conditions.
    The injection volume is 20μL , Use the peak height to plot the concentration of each component in the standard solution
    .


    The absolute amounts of lincomycin, oleandomycin, erythromycin, tilmicosin, tylosin, spiramycin, kititamycin, and josamycin are linear in the range of 0.


    Table 6-33 Linear equations and correlation coefficients of 8 antibiotics

    Under the operating conditions of this method, when the added level of 8 antibiotics is in the range of 2.
    0-50μg/kg, the response value is within the linear range of the instrument, and the signal-to-noise ratio S/N is greater than 5
    .


    According to the sample volume represented by the final sample solution, the constant volume, the injection volume, and the interference during the measurement, it is determined that this method is used to determine the determination of lincomycin, oleandomycin, erythromycin, and erythromycin in puffer fish.


    Related links: Sample pretreatment of 8 kinds of macrolides and lincosamide drug residues in puffer fish and eels

     

     

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