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).
- 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
Definitions
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.
- 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.
- 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 Fertilizer Section 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.