Animals > Livestock Feeds > Trade Memoranda  

T-3-151
GOOD LABORATORY PRACTICES PROTOCOL FOR FEED INGREDIENT APPROVALS

April 13, 1992

Part of the process for clearance of new ingredients/guarantees by the Canadian Food Inspection Agency is the provision by the registrant of an acceptable method of analysis in complete feeds. The following protocol was developed to ensure that the method and test materials provided by the registrant are adequate to allow for expeditious approval of the methodology.

To be included with each submission is a method proven to be specific, selective, reliable, and accurate for the active ingredient in technical products, premixes and formulated products. The following items must be included in the submission to properly evaluate the method(s).

1. The method(s) must be current and in use by the submitting company. The following details must be provided for each method:

a) a clear and concise method description

b) identification of the method performance standards, i.e.

1. percent acceptable recovery
2. analytical range (minimum and maximum)
3. limit of quantitation
4. limit of detection
5. % CV repeatability (within lab)
6. % CV reproducibility (between lab), if available

Definitions - Limit of detection = X + 3 o Limit of quantitation = X + 10o  where X is the average signal of a blank and o is the standard deviation (assumed to be constant at relatively low levels of X).

c) identification of the critical control points and specifications, e.g. evaporation temperature in step 5.3 to be 35° C + 3°C.

d) description of the experimental design used for the method evaluation(s) [evaluation(s) should include recovery studies on a variety of blank feeds at the intended formulation level, with the method of fortification being identified].

e) results of method evaluation(s) to be in tabular form, with statistical analysis.

f) proof of interference study of common drugs and feed additives, and identification of known interferences.

g) chromatograms (if using HPLC or GC) of standards and technical product, and all blanks, feed samples, and premixes used in the method of evaluation(s), and any pertinent comments.

h) raw data and calculated results for the accuracy and precision evaluation of premixes and the various formulated levels of complete feeds that will be manufactured (feeds to contain a variety of ingredients appropriate to the intended species).

2. When the above requirements have been met, the Canadian Food Inspection Agency usually will test the method shown to be most acceptable. When the method is to be tested, the following materials must be supplied.

a) A minimum of five differently formulated complete feeds, i.e. containing a variety of feed ingredients (for each feed, supply a blank and fortified sample), and three premixes in which the ingredient is added (at least 1 kg of each). The amount of ingredient in the samples submitted is to be verified through analysis by the submitting company (the method of analysis used is to be indicated).

b) Five (5) grams of analytical standard and ten (10) grams of 2 lots of technical product, with % purity indicated on the labels.

3. It is desirable that an alternate method be provided to confirm the results (i.e. mass spectrometry, thin layer chromatography, etc.)

4. A trace level procedure that will quantitate 1% of the lowest formulation level of the component must be included when an ingredient/active ingredient is know to be toxic and to certain livestock species.

Once the method(s) has been evaluation, it is desirable to collaboratively study the method.

The method(s) will be incorporated into Laboratory Services Method Manual and therefore be available upon request to the public once the ingredient/guarantee is accepted by the proper authorities.

The Animal Health and Production Division must be informed of any modifications or new methodology. The new or modified methods must be verified by our Laboratory Services Division however, the degree of verification would depend on the effect and changes.

Questions regarding this memorandum may be directed to:

Feed Section
Animal Health and Production Division
Canadian Food Inspection Agency
59 Camelot Drive
Nepean, Ontario   K1A 0Y9
Phone:   (613) 225-2342
Fax:       (613)228-6614