Determination of malonaldehyde in feed - High performance liquid chromatography
1 Scope
This standard specifies a high performance liquid chromatographic method for the determination of malonaldehyde in feed.
This standard is applicable to the determination of malondialdehyde in compound feed, concentrated feed and feed ingredients.
The determination limit of this method is 0.015 mg/kg, and quantitation limit is 0.05 mg/kg.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated reference, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB/T 14699.1 Feeding stuffs - Sampling
3 Principle
Malonaldehyde in the specimen is extracted by trichloroacetic acid and then reacted with thiobarbituric acid (TBA) to generate a pink complex. Collect the supernatant after centrifugation and detect it by high performance liquid chromatography and fluorescence detector, and the content of malonaldehyde should be calculated by external standard method.
4 Reagents
Unless otherwise specified, only recognized analytical reagent and Grade I water specified in GB/T 6682 shall be used for the analysis.
4.1 Acetonitrile: chromatographically pure.
4.2 Potassium dihydrogen phosphate solution (50m mol/L): weigh 6.804 g (accurate to 0.002 g) of potassium dihydrogen phosphate, dissolve it in water and dilute the volume to 1,000 mL.
4.3 Thiobarbituric acid (TBA) solution (0.02 mol/L): weigh 0.288 g (accurate to 0.002 g) thiobarbituric acid in a beaker, add an appropriate amount of water, heat until obtaining a completely dissolved clear solution, cool and then dilute the volume to 100 mL.
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents
5 Apparatus
6 Specimen preparation
7 Analytical procedures
8 Calculation and expression of results
9 Repeatability
Annex A (Informative) Chromatogram of malonaldehyde thiobarbituric acid complex
