The analytical method transfer is regulatory requirement number one. Performed between two companies' testing laboratories -- or it might be even one company with two different sites, or with two laboratories within one company -- the analytical method transfer is a documented process designed to verify a certain laboratory’s capability of performing the analytical testing method’s intended use. Analytical method transfers are performed for validated methods for which complete analytical methods and validation data are available.
4 Common Test Categories for Method Validation Are Defined by USP (an example)
By definition, the common categories of tests for validation are numbered one through four. All these categories are provided by the U.S. Pharmacoepeial Convention (USP) chapter 1225:
Category one covers analytical procedures for quantitation of major components of bulk drug substances or active ingredients (including any preservatives) in finished pharmaceutical products.
Category two covers analytical procedures for determination of impurities in bulk drug substances or degradation compounds in a finished pharmaceutical product. These procedures include quantitative assays and limit tests.
Category three describes analytical procedures for determination of performance characteristics (i.e. dissolution, drug release).
Finally, category four covers Identification tests.
9 Analytical Method Performance Characteritics That Must Be Challenged
The major analytical performance characteristics that should be challenged are as follows:
System Stability
Precision
Intermediate Precision
Regularity
Limits of Detection (LOD)
Limits of Quantification (LOQ)
Specificity
Solution Stability
Some of these categories may be required - or may not be required - depending on the desired results of the analytical method transfer. Analytical method transfers need to be defined and driven by a pre-approved protocol. The method transfer protocol must have clear objectives, should list all necessary materials and analytical procedures to be transferred from the original laboratory site to the receiving site, and should cover the acceptance of the material that it will be assessed against.
Once the method transfer protocol has been executed, the primary report needs to be summarized, written up, and approved by both the receiving laboratory and the transferring laboratory.
Before You Start an Analytical Method Transfer, Be Sure the Method Has Been Previously Validated
Keep in mind that the point of analytical transfers is to have a validated method to transfer. A lot of companies will come to us with a validated method, but one that was validated 20 years ago to completely different standards. The current standard in the industry is the International Conference of Harmonization (ICH), and there are requirements within that group concerning how to specifically validate a method.
While method transfers may be less costly than validation, from time to time it may be necessary to undergo method validation and perhaps develop and validate a new analytical method for a particular, intended purpose.
In certain projects, we’ve had situations where we tried to transfer a product in and we were getting analytical results on the manufactured product, but the QC release results were inconsistent and unreliable. We couldn’t make sense of them. It turned out that the method being transferred wasn’t acceptable for testing the product according to the release specifications. So it was agreed that the QC method had to be re-developed and re-validated. Once that work was performed, that same manufactured product, all of a sudden, fell into line and met all the acceptance criteria and product specification results. But without re-developing and re-validating that method, the product would not have been successfully transferred. From a formulation perspective, it would not have been possible to identify or figure out what was wrong with the formula, if anything was wrong with it. With that being said, it turned out that nothing was wrong with the formula, and rather, it was the QC testing method that it was being tested with. So it’s really, really critical that the analytical methods are developed and validated, prior to performing your analytical method transfer.
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