Oxine copper residual quantity determination method

Oxine copper residual quantity determination method

  • CN 105,699,528 A
  • Filed: 02/15/2016
  • Published: 06/22/2016
  • Est. Priority Date: 02/15/2016
  • Status: Active Grant
First Claim
Patent Images

1. the assay method of a copper 8-hydroxyquinolinate residual quantity, it is characterised in that comprise the following steps:

  • (1) preparation of standard solution;

    weigh copper 8-hydroxyquinolinate standard substance, dissolves and constant volume with methanol, is configured to standard reserving solution, by standard reserving solution stepwise dilution, is configured to series concentration standard working solution;

    (2) extract;

    (i) weighs sample in centrifuge tube, add formic acid acetonitrile solution, homogenizing, centrifugal, collect the first extracting solution;

    (ii) in residue, formic acid solution is added, ultrasonic, centrifugal, collect the second extracting solution;

    (iii) the first extracting solution and the second extracting solution are merged, with formic acid acetonitrile solution constant volume;

    (3) instrument detection;

    after instrument state is stable, with the series concentration standard working solution sample introduction in step (1), LC-MS/MS detects, and on this basis, the sample that step (2) is collected carries out LC-MS/MS detection, wherein,Liquid-phase condition;

    Chromatographic column;

    C18, internal diameter 150mm ×

    2.1mm, 3.5 μ

    m;

    Column temperature;

    40 DEG C;

    Mobile phase;

    0.1% formic acid acetonitrile solution-0.1% formic acid solution (volume ratio is 6;

    4);

    Flow velocity;

    0.2mL/min;

    Sample size;

    5L;

    Mass Spectrometry Conditions;

    Ion source;

    electric spray ion source ESI;

    Scan mode;

    cation scans;

    Detection mode;

    multiple-reaction monitoring pattern;

    Electron spray voltage;

    1000v;

    Sheath atmospheric pressure;

    50Arb;

    Assisted gas pressure;

    10Arb;

    Purge gas;

    1Arb;

    Ion source temperature;

    425 DEG C;

    Transfer tube temperature;

    300 DEG C;

    (4) foundation of standard curve;

    adopting peak area quantification, with sample introduction concentration for abscissa, peak area is vertical coordinate, drawing standard curve;

    (5) interpretation of result;

    calculate the content of copper 8-hydroxyquinolinate in sample as follows

View all claims
    ×
    ×

    Thank you for your feedback

    ×
    ×