0.25% Vitamin D3 (100 IU/mg)

WesleyCrozier
WesleyCrozier
in Instrumentation and Mass Spectrometry
<p>Hello,</p><p></p><p>We're having some trouble with this material.  Currently we're dissolving it in Ethanol (as we are doing with our standard).  Our QC check and QA check (A previously run 0.26% VitD2 material) both come out on target with a deviation of 1.2% and 1.7% respectfully.  However, in our D3 raw material the peak for D3 is so low it's below the calcurve(Area ~1500), roughly 0.00993% consistantly- even after starting again from scratch.  Our sample prep is ~500mg sample in 25mL Ethanol, sonicated for 25 minutes.  The material has reported amounts of vitamin C (which shows up as a large peak in the beginning of this run), Corn starch, and silicon dioxide.  Is this a dissolving issue, if so what might you suggest for dissolving?</p><p></p><p>Thanks,</p><p>Wes</p>

Comments

  • gypsysmom
    gypsysmom

    Hi Wes,

    I checked Sigma for application notes for Vitamin D3.  They have a procedure for extraction fat-soluble vitamins from vitamin tablets:

    http://www.sigmaaldrich.com/etc/medialib/docs/Supelco/Application_Notes/4679.Par.0001.File.tmp/4679.pdf

    Their extraction medium is % acetic acid followed by isopropanol and then using Solid Phase Microextraction.  Even if you don't want to use SPME you could try their extraction procedure.

    Hope this helps.

    Wendy

  • WesleyCrozier
    WesleyCrozier

    Thank you this worked a bit better.  We get about 80% yield using this.  Ill keep playing with it.

  • Hölzer
    Hölzer

    i analyze Ca-d3-tablets the same way. first disregarding with 1% HAc then dilute d3 with iso-propanol, add ACN and cool to -12degree to get out the Ca. but next day the half vial is full of Ca and sorbitol (so i put needle 6mm form vial-bottom to get no problems).

    but to separate the known impurities from the d3 peak i have to use a 5cm and a 15cm-beh column in row (12k-13k PSI). crazy procedure, but it works.

  • WesleyCrozier
    WesleyCrozier

    We've found a solution that works predictably and it's rather simple.  We had ~5mL H2O, shake vigorously, and then dilute with Ethanol.  Apparently the supplier coats the Vitamin D in starch.

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