Difference between revisions of "Summary - vitamin D"

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<p><strong>Scope</strong></p>
 
<p><strong>Scope</strong></p>
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<p>This  European Standard specifies a method for the determination of vitamin  D3 (cholecalciferol) or vitamin D2 (ergocalciferol) in foodstuffs by  high performance liquid chromatography (HPLC).</p>
 
<p>This  European Standard specifies a method for the determination of vitamin  D3 (cholecalciferol) or vitamin D2 (ergocalciferol) in foodstuffs by  high performance liquid chromatography (HPLC).</p>
−
 
−
 
 
<p>Vitamin D3 is primary in foodstuffs of animal origin, while vitamin D2  is primary in wild mushrooms. Both vitamin D3 and vitamin D2 can be  present in fortified foodstuffs. This European Standard is not  applicable for samples with a content of vitamin D3 and vitamin D2.</p>
 
<p>Vitamin D3 is primary in foodstuffs of animal origin, while vitamin D2  is primary in wild mushrooms. Both vitamin D3 and vitamin D2 can be  present in fortified foodstuffs. This European Standard is not  applicable for samples with a content of vitamin D3 and vitamin D2.</p>
−
 
  
 
<p>Apart from the vitamin D activity from the parent forms, vitamin D3 and  vitamin D2, the corresponding metabolites 25-hydroxy vitamin D and  1,25-dihydroxy vitamin D also contribute to the vitamin D activity. This  European Standard does only include measurement of vitamin D3 or  vitamin D2.</p>
 
<p>Apart from the vitamin D activity from the parent forms, vitamin D3 and  vitamin D2, the corresponding metabolites 25-hydroxy vitamin D and  1,25-dihydroxy vitamin D also contribute to the vitamin D activity. This  European Standard does only include measurement of vitamin D3 or  vitamin D2.</p>
−
 
  
 
<p>This European Standard provides the base for the analytical methods. It  is intended to serve as a frame in which the analyst can define his own  analytical work in accordance to the standard procedure.</p>
 
<p>This European Standard provides the base for the analytical methods. It  is intended to serve as a frame in which the analyst can define his own  analytical work in accordance to the standard procedure.</p>
−
 
  
 
<p>This method has been validated in inter-laboratory tests on fortified  and non-fortified samples such as margarine, milk, milk powder, liquid  infant formula, infant formula, cooking oil, and fish oil at levels from  0,4 &micro;g/100 g to 14 &micro;g/100 g.</p>
 
<p>This method has been validated in inter-laboratory tests on fortified  and non-fortified samples such as margarine, milk, milk powder, liquid  infant formula, infant formula, cooking oil, and fish oil at levels from  0,4 &micro;g/100 g to 14 &micro;g/100 g.</p>
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<p><strong>Principal</strong></p>
 
<p><strong>Principal</strong></p>
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−
 
 
<p>Vitamin D3 and vitamin D2 are saponified in the foodstuffs using alcoholic potassium hydroxide solution and extracted by an appropriate solvent. The determination of vitamin D3 or vitamin D2 in an appropriate sample extract solution is carried out by semi-preparative normal phase HPLC followed by reverse phase analytical HPLC.</p>
 
<p>Vitamin D3 and vitamin D2 are saponified in the foodstuffs using alcoholic potassium hydroxide solution and extracted by an appropriate solvent. The determination of vitamin D3 or vitamin D2 in an appropriate sample extract solution is carried out by semi-preparative normal phase HPLC followed by reverse phase analytical HPLC.</p>
−
 
−
 
 
<p>If vitamin D3 is to be determined, then vitamin D2 is used as an internal standard. If vitamin D2 is to be determined, then vitamin D3 is used as an internal standard.</p>
 
<p>If vitamin D3 is to be determined, then vitamin D2 is used as an internal standard. If vitamin D2 is to be determined, then vitamin D3 is used as an internal standard.</p>
−
 
−
 
 
<p>Vitamin D is detected by ultraviolet (UV) spectrometry and peaks are identified on the basis of retention times and additionally by UV spectral profile if diode-array detection is used. The determination is carried out by internal standard procedure using peak areas or peak heights.</p>
 
<p>Vitamin D is detected by ultraviolet (UV) spectrometry and peaks are identified on the basis of retention times and additionally by UV spectral profile if diode-array detection is used. The determination is carried out by internal standard procedure using peak areas or peak heights.</p>
  
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<p><strong>Precision data</strong></p>
 
<p><strong>Precision data</strong></p>
  
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<table>
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<table style="border: 1px solid black;border-collapse: collapse;">
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        <tr style="border: 1px solid black;border-collapse: collapse;" class="tablesorter-headerRow">
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<tr>
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            <th style="border: 1px solid black;border-collapse: collapse;">
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                    <p>&nbsp;</p>
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<th>
 
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<p>&nbsp;</p></th>
 
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<th>
 
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<p> CRM 122<br class="atl-forced-newline" />
 
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Margarine<br class="atl-forced-newline" /> </p></th>
 
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−
<th>
 
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<p> CRM 421<br class="atl-forced-newline" />
 
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Milk powder<br class="atl-forced-newline" /> </p></th>
 
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</tr>
 
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<tr>
 
−
 
 
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<td>
 
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<p> Repeatability standard deviation s<sub>r</sub>, &micro;g/100 g </p></td>
 
−
 
 
−
<td>
 
−
<p> 0,82<br class="atl-forced-newline" /> </p></td>
 
−
 
 
−
<td>
 
−
<p> 0,74<br class="atl-forced-newline" /> </p></td>
 
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</tr>
 
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−
<tr>
 
−
 
 
−
<td>
 
−
<p> Repeatability coefficient of variation, % </p></td>
 
−
 
 
−
<td>
 
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<p> 6,7<br class="atl-forced-newline" /> </p></td>
 
−
 
 
−
<td>
 
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<p> 5,2<br class="atl-forced-newline" /> </p></td>
 
−
</tr>
 
  
−
<tr>
+
            </th>
 +
            <th style="border: 1px solid black;border-collapse: collapse;">
 +
                    <p> CRM 122
 +
                        <br > Margarine
 +
                        <br > </p>
  
−
<td>
+
            </th>
−
<p> Repeatability limit r = [2,8 x s<sub>r</sub>], &micro;g/100 g </p></td>
+
            <th style="border: 1px solid black;border-collapse: collapse;">
 +
                    <p> CRM 421
 +
                        <br > Milk powder
 +
                        <br > </p>
  
−
<td>
+
            </th>
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<p> 2,32<br class="atl-forced-newline" /> </p></td>
+
        </tr>
  
−
<td>
+
        <tr style="border: 1px solid black;border-collapse: collapse;">
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<p> 2,09<br class="atl-forced-newline" /> </p></td>
+
            <td style="border: 1px solid black;border-collapse: collapse;">
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</tr>
+
                <p> Repeatability standard deviation s
−
 
+
                    <sub>r</sub>, µg/100 g </p>
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<tr>
+
            </td>
−
 
+
            <td style="border: 1px solid black;border-collapse: collapse;">
−
<td>
+
                <p> 0,82
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<p> Reproducibility standard deviation s<sub>R</sub>, &micro;g/100 g </p></td>
+
                    <br > </p>
−
 
+
            </td>
−
<td>
+
            <td style="border: 1px solid black;border-collapse: collapse;">
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<p> 0,94<br class="atl-forced-newline" /> </p></td>
+
                <p> 0,74
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+
                    <br > </p>
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<td>
+
            </td>
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<p> 0,78<br class="atl-forced-newline" /> </p></td>
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        </tr>
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</tr>
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        <tr style="border: 1px solid black;border-collapse: collapse;">
−
 
+
            <td style="border: 1px solid black;border-collapse: collapse;">
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<tr>
+
                <p> Repeatability coefficient of variation, % </p>
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+
            </td>
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<td>
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            <td style="border: 1px solid black;border-collapse: collapse;">
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<p> Reproducibility&nbsp;coefficient of variation, % </p></td>
+
                <p> 6,7
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+
                    <br > </p>
−
<td>
+
            </td>
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<p> 7,6<br class="atl-forced-newline" /> </p></td>
+
            <td style="border: 1px solid black;border-collapse: collapse;">
−
 
+
                <p> 5,2
−
<td>
+
                    <br > </p>
−
<p> 5,5<br class="atl-forced-newline" /> </p></td>
+
            </td>
−
</tr>
+
        </tr>
−
 
+
        <tr style="border: 1px solid black;border-collapse: collapse;">
−
<tr>
+
            <td style="border: 1px solid black;border-collapse: collapse;">
−
 
+
                <p> Repeatability limit r = [2,8 x s
−
<td>
+
                    <sub>r</sub>], µg/100 g </p>
−
<p> Reproducibility limit r = [2,8 x s<sub>R</sub>], &micro;g/100 g </p></td>
+
            </td>
−
 
+
            <td style="border: 1px solid black;border-collapse: collapse;">
−
<td>
+
                <p> 2,32
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<p> 2,66<br class="atl-forced-newline" /> </p></td>
+
                    <br > </p>
−
 
+
            </td>
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<td>
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            <td style="border: 1px solid black;border-collapse: collapse;">
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<p> 2,21<br class="atl-forced-newline" /> </p></td>
+
                <p> 2,09
−
</tr>
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                    <br > </p>
 +
            </td>
 +
        </tr>
 +
        <tr style="border: 1px solid black;border-collapse: collapse;">
 +
            <td style="border: 1px solid black;border-collapse: collapse;">
 +
                <p> Reproducibility standard deviation s
 +
                    <sub>R</sub>, µg/100 g </p>
 +
            </td>
 +
            <td style="border: 1px solid black;border-collapse: collapse;">
 +
                <p> 0,94
 +
                    <br > </p>
 +
            </td>
 +
            <td style="border: 1px solid black;border-collapse: collapse;">
 +
                <p> 0,78
 +
                    <br > </p>
 +
            </td>
 +
        </tr>
 +
        <tr style="border: 1px solid black;border-collapse: collapse;">
 +
            <td style="border: 1px solid black;border-collapse: collapse;">
 +
                <p> Reproducibility&nbsp;coefficient of variation, % </p>
 +
            </td>
 +
            <td style="border: 1px solid black;border-collapse: collapse;">
 +
                <p> 7,6
 +
                    <br > </p>
 +
            </td>
 +
            <td style="border: 1px solid black;border-collapse: collapse;">
 +
                <p> 5,5
 +
                    <br > </p>
 +
            </td>
 +
        </tr>
 +
        <tr style="border: 1px solid black;border-collapse: collapse;">
 +
            <td style="border: 1px solid black;border-collapse: collapse;">
 +
                <p> Reproducibility limit r = [2,8 x s
 +
                    <sub>R</sub>], µg/100 g </p>
 +
            </td>
 +
            <td style="border: 1px solid black;border-collapse: collapse;">
 +
                <p> 2,66
 +
                    <br > </p>
 +
            </td>
 +
            <td style="border: 1px solid black;border-collapse: collapse;">
 +
                <p> 2,21
 +
                    <br > </p>
 +
            </td>
 +
        </tr>
 
</table>
 
</table>
−
 
  
 
<p>Results obtained in 1994.</p>
 
<p>Results obtained in 1994.</p>

Latest revision as of 13:33, 9 May 2019

EN 12821 Foodstuffs - Determination of vitamin D by high performance liquid chromatography - Measurement of cholecalciferol (D3) or ergocalciferol (D2):


Scope

This European Standard specifies a method for the determination of vitamin D3 (cholecalciferol) or vitamin D2 (ergocalciferol) in foodstuffs by high performance liquid chromatography (HPLC).

Vitamin D3 is primary in foodstuffs of animal origin, while vitamin D2 is primary in wild mushrooms. Both vitamin D3 and vitamin D2 can be present in fortified foodstuffs. This European Standard is not applicable for samples with a content of vitamin D3 and vitamin D2.

Apart from the vitamin D activity from the parent forms, vitamin D3 and vitamin D2, the corresponding metabolites 25-hydroxy vitamin D and 1,25-dihydroxy vitamin D also contribute to the vitamin D activity. This European Standard does only include measurement of vitamin D3 or vitamin D2.

This European Standard provides the base for the analytical methods. It is intended to serve as a frame in which the analyst can define his own analytical work in accordance to the standard procedure.

This method has been validated in inter-laboratory tests on fortified and non-fortified samples such as margarine, milk, milk powder, liquid infant formula, infant formula, cooking oil, and fish oil at levels from 0,4 µg/100 g to 14 µg/100 g.

Principal

Vitamin D3 and vitamin D2 are saponified in the foodstuffs using alcoholic potassium hydroxide solution and extracted by an appropriate solvent. The determination of vitamin D3 or vitamin D2 in an appropriate sample extract solution is carried out by semi-preparative normal phase HPLC followed by reverse phase analytical HPLC.

If vitamin D3 is to be determined, then vitamin D2 is used as an internal standard. If vitamin D2 is to be determined, then vitamin D3 is used as an internal standard.

Vitamin D is detected by ultraviolet (UV) spectrometry and peaks are identified on the basis of retention times and additionally by UV spectral profile if diode-array detection is used. The determination is carried out by internal standard procedure using peak areas or peak heights.


Precision data

 

CRM 122
Margarine

CRM 421
Milk powder

Repeatability standard deviation s r, µg/100 g

0,82

0,74

Repeatability coefficient of variation, %

6,7

5,2

Repeatability limit r = [2,8 x s r], µg/100 g

2,32

2,09

Reproducibility standard deviation s R, µg/100 g

0,94

0,78

Reproducibility coefficient of variation, %

7,6

5,5

Reproducibility limit r = [2,8 x s R], µg/100 g

2,66

2,21

Results obtained in 1994.


Data derived from EN 12821.

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