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Chapter 6 - Sampling and Laboratory Requirements
6.2 Good Laboratory Practices Protocol for Feed Ingredient Approvals

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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).

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 + 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).

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

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.

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 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.

Guidelines for the Evaluation of Methods to Determine the Viability of Direct Fed Microbials and Forage Additives containing Viable Microorganisms

Part of the process for registration of direct fed microbials or forage additives containing viable microorganisms by the CFIA is the provision by the applicant of an acceptable method of analysis for the microorganisms in the carrier or filler. The applicant is also required to provide the necessary data to support reliability of the method. The following protocol is intended to ensure that the method, data and test materials provided by the applicant are adequate to allow for expeditious evaluation, validation and approval of the methodology.

1. Method Format

The purpose of the method submission is to permit the verification of label claims and to allow the evaluator and analyst to understand and perform the method exactly as the originator intended. It is therefore necessary that the method contains all the necessary information presented in a detailed step-by-step standard operating procedure.

The method submitted must be clear and concisely written, currently in use by the submitting company, and proven to be specific, selective, reliable, and accurate for the enumeration of viable microorganisms in formulated products. Critical control points, specifications for quality control and familiarization must be included in the methodology.

The following supporting documents for method performance standards must be included in the submission to properly evaluate the method:

2. Supporting Data

The applicant must provide the following information in support of the proposed methodology, which includes raw data and statistical analyses from their own method evaluation (data should be presented in a tabular form):

3. CFIA Laboratory Evaluation

When the above requirements are met, CFIA will proceed with a desk review followed by a laboratory evaluation of the method. For the laboratory evaluation, the following materials must be supplied by the company.

4. Evaluation Criteria

An adequate method for the enumeration of the microorganism(s) will be approved following criteria based on specificity, accuracy, precision, repeatability and reproducibility, taking into consideration the analytical results provided by the company and those generated by CFIA.

5. CFIA Report

Upon request, the CFIA will prepare a report including the following information:

6. Changes to Methodology

The CFIA must be informed of any modifications of the methodology. The new or modified method must be submitted to a desk review. The degree of verification will depend on the changes.

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