A kind of detection method of vitamin B6 residual solvent

A kind of detection method of vitamin B6 residual solvent

  • CN 107,300,591 A
  • Filed: 06/30/2017
  • Published: 10/27/2017
  • Est. Priority Date: 06/30/2017
  • Status: Active Application
First Claim
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1. a kind of detection method of vitamin B6 residual solvent, it is characterised in that this method comprises the following steps:

  • A, solution are preparedEthanol storing solution:

    Precision weighs ethanol 2.5g into 100ml volumetric flasks, and quarter is diluted to 50% dimethyl sulphoxide aqueous solutionDegree, is mixed.Toluene storing solution:

    Precision weighs benzene 0.445g into 100ml volumetric flasks, and quarter is diluted to 50% dimethyl sulphoxide aqueous solutionDegree, is mixed.Benzene storing solution:

    Precision weighs benzene 100mg into 100ml volumetric flasks, and scale is diluted to 50% dimethyl sulphoxide aqueous solution,Mix.Precision measures 1ml into 100ml volumetric flasks, and scale is diluted to 50% dimethyl sulphoxide aqueous solution, mixes.Standard Stock solutions:

    Precision measures ethanol storing solution 10ml, toluene storing solution 10ml, benzene storing solution 10ml and puts 100ml appearancesIn measuring bottle, scale is diluted to 50% dimethyl sulphoxide aqueous solution, is mixed.Standard liquid:

    Precision measures standard reserving solution 10ml and put in 100ml volumetric flasks, is diluted with 50% dimethyl sulphoxide aqueous solutionTo scale, mix.Produce the μ

    g/ml of ethanol 250, the μ

    g/ml of toluene 44.5, the μ

    g/ml of benzene 0.1.Standard items test solution:

    Precision is measured in 5.0ml standard liquids, top set empty bottle, closed, is mixed.Need testing solution:

    Precision weighs 0.25g vitamin B6 samples, is placed in ml headspace bottle, plus 50% dimethyl sulfoxide 5.0ml moltenSolution, seal bottle cap.Blank solution:

    Take in 50% dimethyl sulfoxide aqueous solution 5.0ml top set empty bottles, seal bottle cap.System suitability solution:

    Pipette in 5.0ml standard liquids, top set empty bottle, seal bottle cap, mix.B, system suitability test:

    Stable more than the 60min of system, sample introduction blank solution is confirmed in collection of illustrative plates without other impurities;

    Several pins can be entered as needed empty moreIn vain.Standard liquid head space 1.0ml is taken, the separating degree recorded between chromatogram, each chromatographic peak is not less than 1.5;

    It is required that being:

    RepeatThe peak area RSD at 6 each residual solvent correspondence peaks of sample introduction should be not more than 10%, and theoretical cam curve is not less than 5000.C, assay method:

    Standard items are taken to test solution, need testing solution head space 1.0ml, sample introduction analysis in the following order respectively:

    After blank solution inserting needle, six needle system adaptability solution are entered successively, enters two pin standard items test solution, enter a pin test sampleSolution, enter again a pin need testing solution, enter a pin standard items test solution, chromatogram is recorded respectively.

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