Method Validation / Reference Standards
Download more than 350 documents: SOPs, examples, templates, checklists,
FDA waning letters, 483 inspectional observations, FDA and other official
guidelines, presentations/publications from FDA personnel.
S-115
The FDA requires that an investigation be conducted whenever an
Out-of-Specification (OOS) result is observed. This SOP defines the
requirements for dealing with OOS results. Even if a batch is rejected based
on an OOS result, the investigation is necessary to determine if the result
is associated with other batches of the same drug product or other products.
This SOP deals with results that fall outside the specifications or
acceptance criteria established in new drug applications, official
compendia, or by the manufacturer and suspect within test results. The SOP
applies to OOS as a result of analytical errors, process errors and
manufacturing errors.
S-116
S-268
Electronic Laboratory Notebooks (ELN) are frequently used in regulated
development and QC laboratories. The purpose of this operating procedure is
to ensure that ELNs used in regulated environments comply with regulations .
Following this SOP does not mean that users comply with all regulations in
all aspects. The procedure applies whenever Electronic Laboratory Notebooks
are used in a regulated environments
S-509
S-511
S-613
Follow this step-by-step SOP to develop and document your
chromatographic method. It includes validation parameters and
examples for acceptance limits.
S-614
Accurate and consistent analytical data can only be obtained with
validated methods. When validated methods are transferred between
laboratories and sites, their validated state should be maintained to ensure
the same reliable results in the receiving laboratory. This SOP addresses
the process for transferring validated analytical methods.
S-615
S-617
S-662
E-116
E-158
Laboratory computer systems used in regulated environments should be
validated and well controlled. This form helps to identify qualification and
validation requirements for software and computer systems
E-164
E-171
E-176
E-184
Use this checklist to audit your laboratory. It is also most useful to
learn what 3rd party auditors and regulatory inspectors will look at.
E-781-02
A-552
A-603
Published in LC/GC Magazine. Reference paper with advice when, what and
how to validate and revalidate analytical methods. Takes into account USP
and ICH guidelines.
A-605
Published in BioPharm. This paper gives a strategy for the validation of
HPLC methods developed in house and a recommendation on the implementation.
It also recommends a list of documents that should be produced during, and
on completion of, validation.
A-607
Published in PharmTech. The paper answers a frequent question: do I need
to validate Standard methods, such as USP, ASTM or ISO., and if so what
should be validated and how
A-633
Published in BioPharm. This paper gives recommendations for the
preparation of reference materials and how to implement a quality assurance
program for purchased and home made reference standards.
A-635
This article from Carl Craig, Ph.D., General Manager,
Pharmaceutical Resource Associate explains the concept of traceability and
gives practical examples on how in implement traceability in chemical
measurement
P-561
Design, Conduct and Document for Efficiency and Compliance.
F-505
Draft
F-507
G-262
Yvonne McKnight, chemist at the FDA Philadelphia gave a presentation at
the IVT conference "Laboratory Controls & Compliance" in Philadelphia on
April 11, 2005. More than 120 delegates listened to the presentation
entitled: Inspection Issues in the Analytical Laboratory: An FDA
Perspective". During the presentation McKnight quoted and discussed FDA
regulations and enforcement activities, she gave advice on how to prepare
for FDA inspections and reported on recent trends and statistics of
inspectional deviations. Highlight of the presentation was a TOP TEN list
with 483 inspectional observations.
G-263
Sybil Wellstood, Ph.D., of FDA CDRH Division of Bioresearch monitoring
gave a presentation on FDA's Bioresearch and In Vitro Diagnostics. The
objective was to provide an overview of the CDRH Bioresearch monitoring
program (BIMO) and to discuss how the BIMO program applies to in vitro
diagnostic (IVD) studies conducted under 510(k) pre-market notifications.
One of the responsibilities of the Office of Compliance is to develop and
issue inspection assignments to field offices, to evaluate and classify
Establishment Inspection reports and to initiate follow-up regulatory
actions and correspondence. In line with this responsibility Dr. Wellstood
gave an insight on FDA inspections: the inspection process, whom they
inspect, their expectations, type of inspections and how an inspections is
conducted, concluded and followed up. An FDA 483 form report is written
right after the inspection with deviations from regulations. Deviations from
guidelines do not appear on the Form FDA-483, but may be included in the
discussion" she said. She also recommended to respond verbally during the
final discussion and/or sent a written response to District Office.
G-268
A Regulatory Perspective by Patrick J. Faustino, Ph.D, Office of
Pharmaceutical Science, Analytical Methods Technical Committee, Center for
Drug Evaluation and Research, U.S. Food and Drug Administration.
Shows the direction of the FDA towards method validation practices.
G-334
G-425
Presented by William B. Furman from the US FDA. This question comes
frequently when methods are transferred from development to manufacturing or
when the equipment manufacturer is changed. Examples are HPLC flow rate, pH
of mobile phase, column temperature and others.
G-427
A Regulatory Perspective by Patrick J. Faustino, Ph.D, Office of
Pharmaceutical Science, Analytical Methods Technical Committee, Center for
Drug Evaluation and Research, U.S. Food and Drug Administration.
Shows the direction of the FDA towards method validation practices.