Good Laboratory Practices Protocol for Fertilizer and Supplement Registrations
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Part of the process for registration of new fertilizers and supplements by the Canadian Food Inspection Agency is the provision by the registrant of an acceptable method of analysis of the product. 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 the 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 clear and concise method description;
- identification of the method performance standards, i.e.;
- percent acceptable recovery
- analytical range (minimum and maximum)
- limit of quantitation
- limit of detection
- % CV repeatability (within lab)
- % CV reproducibility (between lab), if available
Limit of detection = x + 3ó
Limit of quantitation = x + 10ó
where x is the average signal of a blank and ó is the standard deviation (assumed to be constant at relatively low levels of X);
- identification of the critical control points and specifications, e.g. evaporation temperature in step 5.3 to be 35°C ± 3°C;
- description of the experimental design used for the method evaluation(s) [evaluation(s) should include recovery studies on a variety of blank samples at the intended formulation level, with the method of fortification being identified];
- results of method evaluation(s) to be in tabular form, with statistical analysis;
- proof of interference study and identification of known interference;
- chromatograms (if using HPLC or GC) of analytical standards, technical product, blanks and formulated product used in the method evaluation(s), and any pertinent comments;
- raw data and calculated results for the accuracy and precision evaluation of the various formulated levels of the product that will be manufactured.
2. When the above requirements have been met, the Canadian Food Inspection Agency will usually test the method shown to be most acceptable. When the method is to be tested, the following materials must be supplied:
- a minimum of five samples of the formulated product(s). The amount of active ingredient in the samples submitted is to be verified through analysis by the submitting company (the method of analysis used is to be indicated);
- 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.).
Once the method(s) has been evaluated, it is desirable to collaboratively study the method.
The Canadian Food Inspection Agency must be informed of any modifications or new methodology. The new or modified methods must be verified; however, the degree of verification would depend on the effect and changes.
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