Chapter 6 - Sampling and Laboratol)r Requirernents

6.:2 Good Laboratory Practices Protocol for

~eed -~~redien~ Approvals

This a.9e is art of the Guidance Document R~epo1sito~_.__

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Introduction:
Part of the process for clearance of new ingredients/guarantees by the CFIA 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).
Part 1.
The method(s) must be current and in use by the submitting company. The following details
must be provided for each method:

1. a clear and concise method description

2. 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. % coefficient of variation (CV) repeatability (within lab)
6. % CV reproducibility (between labs), if available

Definitions
Limit of detection= X + 3o
Limit of quantitation = X + 1Oo
where Xis the average signal of a blank and o is the standard deviation (assumed to
be constant at relatively low levels of X).
 3. identification of the critical control points and specifications, for example ' 'evaporation
temperature in step 5.3 to be 35C 3C".

4. 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]

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

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

7. 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.

8. 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).

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

1. 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)
 2. Five (5) grams of analytical standard and ten (10) grams of 2 lots of technical product,
with % purity indicated on the labels.

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

Part 4.
A trace level procedure that will quantitate 1% of the lowest formulation level of 1he
component must be included when an ingredient/active ingredient is know to be toxic to
certain livestock species.
Once the method(s) have been evaluated, it is desirable to collaboratively study the method.
The method(s) will be incorporated into the Laboratory Services Method Manual and will
therefore be available upon request to the public, once the ingredient/guarantee is accepted by
the proper authorities.

The Animal Feed Division must be informed of any modifications or new methodology. The
new or modified methods must be verified by our Science Branch, however the degree of
verification would depend on the effect and changes that are required in the methodology.

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