1 Scope
This standard specifies the determination methods of Vitamins A, E and D in foods.
Method I of this standard is applicable to the determination of Vitamins A and E in foods.
Method II of this standard is applicable to the determination of Vitamins E in foods such as edible oil, nuts, beans and chili powder.
Method III of the standard is applicable to the determination of Vitamins D2 and D3 in foods.
Method IV of this standard is applicable to the determination of Vitamins D2 and D3 in formula foods.
Method I Determination of Vitamins A and E in Foods Reversed-phase High Performance Liquid Chromatography
2 Principle
After subjecting to saponification (subjecting to enzymolysis with amylase first for starch-containing specimen), extraction, purification and concentration, Vitamins A and E in the specimen are separated by C30 or PFP reversed-phase liquid chromatographic column, detected with ultraviolet detector or fluorescence detector and quantitated by external standard method.
3 Reagents and Materials
Unless otherwise specified, analytically-pure reagents and Grade I water (defined in GB/T 6682) are adopted for the purposes of this method.
3.1 Reagents
3.1.1 Absolute ethanol (C2H5OH): without aldehyde substance after inspection, see A.1 for inspection method.
3.1.2 Ascorbic acid (C6H8O6).
3.1.3 Potassium hydroxide (KOH).
3.1.4 Ethyl ether [(CH3CH2)2O]: without peroxide after inspection, see A.2 for inspection method.
3.1.5 Petroleum ether (C5H12O2): with boiling range of 30℃~60℃.
3.1.6 Anhydrous sodium sulfate (Na2SO4).
3.1.7 pH test paper (at the pH range of 1~14).
3.1.8 Methanol (CH3OH): chromatographically pure.
3.1.9 Amylase: activity unit≥100U/mg.
3.1.10 2,6-Di-tert-butyl-4-methylphenol (C15H24O): referred to as BHT.
3.2 Reagent preparation
3.2.1 Potassium hydroxide solution (50g/100g): weigh 50g of potassium hydroxide, dissolve it with 50mL of water, after cooling, store it in a polyethylene bottle.
3.2.2 Petroleum ether - ethyl ether solution (1+1): measure 200mL of petroleum ether and add into 200mL of ethyl ether, mix them well.
Contents
Foreword i
1 Scope
2 Principle
3 Reagents and Materials
4 Apparatuses
5 Analysis Procedures
6 Expression of Analysis Results
7 Accuracy
8 Others
9 Principle
10 Reagents and Materials
11 Apparatuses
12 Analysis Procedures
13 Expression of Analysis Results
14 Accuracy
15 Others
16 Principle
17 Reagents and Materials
18 Apparatuses
19 Analysis Procedures
20 Expression of Analysis Results
21 Accuracy
22 Others
23 Principle
24 Reagents and Materials
25 Apparatuses
26 Analysis Procedures
27 Expression of Analysis Results
28 Accuracy
29 Others
Appendix A
Appendix B Calibration Method for Concentrations of Vitamins A, D and E Standard Solutions
Appendix C Chromatogram