Chemistry Reference
In-Depth Information
tAble 1.3
Information typically Included in an Analytical procedure description
section
comments
Principle
A statement of the principle or objective of the procedure: for example,
isocratic reversed-phase HPLC separation with UV detection
Sampling
Number of samples, how they are used, number of replicates per sample
Equipment and Parameters
Listing of all equipment (type, detector, column type/dimensions) and
parameters (temperature, flow rate, wavelength) used
Reagents
List reagents and their grade, directions for preparation, storage
conditions, shelf life, directions for safe use,
System Suitability Testing
Per USP Chapter 621 for chromatography, acceptance criteria are
predefined and demonstrate that the system is in working order at the
time of the analysis
Preparation of Standards
Procedures for the preparation of all standards (e.g., stock, working
standards, internal standards) should be included
Preparation of Samples
Sample preparation should be clearly described, including any specific
details for specialized sample preparation (e.g., derivatization, solid
phase extraction) procedures
Procedure
A step-by-step description of the procedure should be provided,
including injection sequences, start-up parameters, and equilibration
times if appropriate.
Calculations
Representative calculations defining all symbols, constants, etc. Any
formulas or transformations should be described in detail.
Reporting of Results
General:
Procedures for Impurities:
The format used to report results
(e.g., % label claim, v/v, w/w,
parts per million (ppm)) should
be specified.
Include the name and location
identifier (e.g., relative retention
time (RRT)), type of impurity,
and detection or quantitation
limit if appropriate.
Samples shipped from outside the United States should contain the appropriate
customs forms to reduce delay in delivery. If special storage precautions (e.g., freez-
ing, use of an inert gas blanket) are required to protect sample integrity, arrange-
ments should be made in advance with the validating laboratory for scheduled direct
delivery. If a sample is toxic or potentially hazardous, the container should be promi-
nently labeled with an appropriate warning and precautionary handling instructions.
1.5.6.2 responsibilities
It is the responsibility of the applicant to provide complete contact information, for
FDA contact, sample requests, etc. The FDA review chemist evaluates the application
and in coordination with the appropriate FDA laboratory contacts applicants regard-
ing the nowadays unlikely event that a method is actually replicated in the FDA labo-
ratories. The laboratory also communicates any results and comments to the review
chemist. Finally, the investigator has the responsibility to inspect the laboratory
where the release and stability testing are performed to ensure compliance with GMP.
