View Report Details

The Determination of Vitamin D3 in Feeds and Petfoods

Project Code: F01003

30/07/2003

LGC
Lawrance, P

Vitamin D3 is a permitted additive in petfood and animal feed and is controlled by the Feeding Stuffs Regulations 2000 and its amendments.

The Feeding Stuffs (Sampling and Analysis) Regulations 1999 specifies analytical methods to be used for the determination of additives in animal feeding stuffs, however there is no official method for the determination of vitamin D3. The use of different methods can give rise to differences in results between laboratories, potentially causing disputes and requiring the prescription of wide tolerances in the legislation.

LGC was contracted by the Food Standards Agency to develop an optimised HPLC procedure for the determination of vitamin D3 in animal feeds and petfood and to validate this procedure by collaborative trial.

LGC formed a consortium of four laboratories to evaluate and optimise an HPLC procedure following on from work carried out under the auspices of the Royal Society of Chemistry Analytical Methods Committee (Feeding Stuffs sub-committee). Potential methods were evaluated and an optimised procedure was developed. Following a successful pilot trial, the method was validated by collaborative trial.

Six petfood or animal feed materials were chosen by the consortium to represent a range of feed/petfood matrices and a range of vitamin D3 concentrations. These were then prepared and tested for homogeneity and stability at LGC.

Fifteen laboratories from the UK and EU states were selected for participation in the collaborative study. Participants were sent twelve coded samples (six blind duplicates) to be analysed once only and a further six samples to be spiked on analysis in order to assess analyte recovery. A practice sample with known vitamin D3 concentration was also provided. Results were subjected to statistical evaluation according to IUPAC recommendations6. Repeatability and reproducibility data are shown below. Horrat values were calculated for each material and ranged between 0.7 and 2.3, therefore the performance of the method was acceptable in all materials.

Summary of collaborative study data for petfood and animal feed

	Cattle concentrate	Poultry feed	Cattle/pig feed	Semi-dry cat food	Dog food	Guinea Pig mix
Mean (μg/kg)	16.50	9.44	4.81	5.43	0.74	4.60
s_r	0.858	0.784	0.763	1.016	0.042	0.937
RSD_r (%)	5.2	8.3	15.9	18.7	5.7	20.4
r	2.40	2.19	2.14	2.84	0.12	2.62
s_R	2.375	2.474	1.230	1.050	0.365	1.234
RSD_R (%)	14.4	26.2	25.7	19.3	49.6	26.9
R	6.65	6.93	3.45	2.94	1.02	3.46
Ho_R	0.7	1.2	1.2	0.8	2.3	1.2

Main File

Some of the files on this site may be in a format that your computer can't read. However, you can download Readers and Viewers for the following document types below: