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Laboratory Compliance

Download more than 500 documents: SOPs, examples, templates, checklists, FDA waning letters, 483 inspectional observations, FDA and other official guidelines, presentations/publications from FDA personnel.

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FDA Presentation
Quality by Design Approaches to Analytical Methods - FDA Perspective

G-428

Yubing Tang, Ph.D., FDA/CDER/ONDQA, AAPS, Washington DC
Shows the direction of the FDA towards Quality by Design Approaches  for analytical method validation. Most useful are the life-cycle process and examples for implementation.

 

Standard Operating Procedures

SOP
Internal Audits – Preparation, Conduct, Follow-up

S-108 

 

SOP
Corrective and Preventive Actions

S-114

 

SOP
Handling Out-of-Specification Results

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.

 

SOP
Handling Out-of-Trend Results

S-116

 

SOP
Out of Specifications Data Trending

S-117

 

SOP
Training for GLP Compliance

S-123

 

SOP
Validation of Spreadsheet Applications

S-264

Quality standards, regulatory agencies and some company policies require software used for evaluation of critical data to be properly validated. Spreadsheet applications are considered as software and should be validated to demonstrate suitability for their intended use. The purpose of this operating procedure is to ensure that Spreadsheet applications are validated during their development and installation and periodically reevaluated during operation.

 

SOP
Using Macros and Spreadsheets (M&S) in a Regulated Environment

S-265

 

SOP
Development and Use of Spreadsheets in Part 11 and GxP Environments

S-266  

 

SOP
Validation of Electronic Laboratory Notebooks
S-267

 

SOP
Using Electronic Laboratory Notebooks in FDA Regulated Environments

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  

 

SOP
Retention and Archiving of Electronic Records

S-315

Regulations and company policies require records to be available for up to 10 or more years. Ensuring the authenticity, reliability and long-term availability of electronic records is challenging because they can be easily altered. This procedure should help to reliably maintain and retain electronic records over the entire retention period. It applies to the entire retention period of records as required by applicable regulations and company policies.

 

SOP
Scanning of Paper Records for ISO 17025 Compliant Archiving
316-02

 

SOP
 Setting up a Quality System for Pharmaceutical Testing Laboratories

S-503

 

SOP
Internal Audits for ISO 17025

S-507

 

SOP
Change Control of Analytical Equipment

S-509

 

SOP
Conducting Laboratory Management Review

S-510

 

SOP
Auditing Analytical Laboratories

S-511

 

SOP
Auditing Laboratories for ISO 17025 Compliance

S-511-02

 

SOP
Auditing Quality Control Laboratories

S-511-03

 

SOP
Review and Approval of Analytical Test Results

S-512

 

SOP
Training for Laboratory Personnel

S-513

 

SOP
Purchasing and Receipt of Supplies for Laboratories

S-514

 

SOP
Purchasing of Services for Laboratories

S-514-02

 

SOP
Quality Assessment of Laboratory Service Providers

S-515-02

 

SOP
Risk Assessment for Laboratory Systems

S-519

 

SOP
Laboratory Complaint Handling for ISO 17025

S-520-01

 

SOP
Improving the Effectiveness of the Laboratory Management System

S-520-11

 

SOP
Laboratory Facilities and Environmental Control

S-520-16

 

SOP
 Providing Services to Customers
S-526

For ISO 17025 Compliance

 

SOP
 Identification and Control of Laboratory Records

S-526

 

SOP
Preparation of Laboratory Working Standards
S-532

 

SOP
Reserve Samples in Laboratories

S-535

 

SOP
Measurement Uncertainty in Chemical Analysis
S-536

 

SOP
Measurement Traceability in Chemical Analysis

S-537

 

SOP
Maintenance of Laboratory Equipment

S-541

 

SOP
Selection of Analytical Methods and Procedures

S-605

 

SOP
Review of Analytical Methods and Procedures

S-605-02

 

SOP
Development and Validation of Analytical Methods through Quality by Design

S-609

 

SOP
Validation of HPLC Methods
S-611

 

SOP
Transfer of Analytical Methods

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.

 

SOP
Verification of Compendial Methods

S-615

 

SOP
Change versus Adjustment of Compendial Methods

S-617

 

 

SOP
Validation of Stability Indicating Methods
S-619

 

SOP
Procedures and Deliverables for Qualification of USP <1058> Instrument Categories

S-630

 

 

SOP
Qualification of Analytical Equipment

S-632

 

 

SOP
Requalification of Analytical Equipment

S-633

 

SOP
Developing and Maintenance of Test Scripts for Analytical Systems

S-635

 

SOP
Calibration and Qualification of Stability Chambers

S-652

 

SOP
Performance Testing of Stability Chambers

S-653

 

SOP
Risk Based Validation of Laboratory Computer Systems

S-662

 

SOP
Retrospective Validation of Laboratory Computer Systems

S-663

Templates / gap analyses / checklists / case studies / examples

Checklist
Out of Specification Situations (OOS)

E-116

 


Out of Trend Situations

E-118

 

Checklist
Shelf Life Testing for Drugs and Drug Substances

E-135

 

Checklist
Security and Integrity of Electronic Data in Laboratories

E-148-03

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

 

Checklist
Using Macros and Spreadsheets in a Regulated Environment

E-156

 

Checklist
Validation of Analytical Methods

E-171

 

Checklist
Validation of Analytical Methods according to the FDA Guidance 2014

E-171-02

 

Checklist
Review of Analytical Methods and Procedure

E-171-03

 

Checklist
Verification of Compendial Methods
E-174

 

Checklist
ISO 17025
E-178

 

Checklist
 Sampling and Sample Handling

E-179

 

Checklist
Laboratory audit

E-184

 

Checklist
Auditing Quality Control Laboratories

E-184-03

Use this checklist to audit your Quality Control laboratory and contract laboratories. It is also most useful to learn what 3rd party auditors and regulatory inspectors will look at.

 

Checklist
Pharmaceutical Analytical Laboratory QA Audit
E-184-05

 

Checklist
Measurement Uncertainty in Chemical Analysis

E-186

 

Checklist
Measurement Traceability in Chemical Analysis

E-187

 

Example
30 Test Procedures for Laboratory Equipment:
For Operational Performance and Compliance

E-363

 

Case Studies
How to Respond to 483s and Warning Letters Related to OOS and Failure Investigations
E-417

 

Case Studies
Matrixing and Bracketing in Stability Studies

E-431

 

Case Studies
Verification of Compendial Procedure

E-450-01

 

Case Studies
Risk Based Methodologies for Laboratory Tasks

E-453

 

Checklist
Using Computer Systems in ISO 17025 Environments

E-610

 

Case Studies
Elemental Impurity Analysis According to USP <232/233>

E-611

 

Checklist
Compliance for Biopharmaceutical Laboratories 

E-616-01

 

Example
Risk Assessment - HPLC System - HPLC System

E-711-03

 

Example
Installation Qualification HPLC System

E-711-07

 

Example
Performance Qualification - HPLC System

E-711-09

 

Example
Test Sheet and Approvals HPLC System

E-711-12

 

Example
Design Qualification SFC System

E-716-05

 

Example
Validation Report SFC System 

E-716-11

 

Example
Qualification Plan - Stability Chambers

E-721-01

 

Example
Risk Assessment Stability Chambers  

E-721-03

 

Example
Performance Qualification - Stability Chambers

E-721-09

 

Example
Validation Plan - Validation of HPLC Methods

E-731-21

 

Example
Validation Report:: Assay of Drug Substances in Drug Products by HPLC

E-731-34

 

Example
Requirement Specifications Spreadsheet Applications

E-745-02

 

Example
Step-by-Step Validation - Chromatography Data System

E-781-00

 

Example
Validation Project Plan - Chromatography Data System -
E-781-01

 

Example
Supplier Assessment - Chromatography Data System

E-781-04

 

Example
Test Plan - Chromatography Data System

E-781-06

 

Example
 Installation Qualification - Chromatography Data System

E-781-07

 

Example
 Performance Qualification – Chromatography Data System

E-781-09

 

Form
Horizontal Laboratory Audit

K-1111

 

Form
Reporting Analytical Results with Expanded Uncertainty

K-1664

 

Form
Documenting Corrective Actions

K-3511

 

Form
Documenting Corrective Actions

K-3511

 

Form
Project Plan for ISO 17025
K-1545

 

Master Plan
Master Plan: Stability Studies for Drugs and Drug Substances

M-168

 

Master Plan
Master Plan: Stability Studies for Drugs and Drug Substances

M-168

 

Master Plan
Development and Validation of Analytical Methods through QbD

M-190

 

References
33 Computer and Software Clauses in ISO 17025 - And recommendations for Implementation

R-201

 

Reference papers and presentations, private authors

 

Journal publication
Reference Paper: (Laboratory) Equipment Qualification and Computer System Validation

A-552

 

Journal publication
Qualification of High-Performance Liquid Chromatography Systems, Published in BioPharm

A-553

 

Reference Paper
Qualification and validation of software and computer systems in laboratories,
Part 3: Installation and Operational Qualification

A-558.

 

Reference Paper
Validation of Analytical Methods: Review and Strategy

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.

 

Reference Paper
Validation of HPLC Methods

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.

 

Reference Paper
Validation of Standard Methods

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

 

Reference Paper
Preparation and Qualification of Certified Reference Material and Working Standards.

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.

 

Reference Paper
Traceability of Analytical Measurements

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

 

 

Presentation
Validation in Laboratories

Nick Buhay, Ludwig Huber

P-503

 

Presentation
Handling Out-of-Specification Tests Results and Failure Investigations

 Ludwig Huber

P-505

 

Presentation
Quality Assurance and Compliance in Laboratories

 Ludwig Huber

P-506

 

Presentation
Crafting an Efficient & Cost-effective Lab Compliance Program

 Ludwig Huber

P-509

 

Presentation
Analytical Instrument Qualification

Horacio Pappa, USP

P-517

 

Presentation
Effective Verifiction of Compendial Methods

 Ludwig Huber

P-518

Design, Conduct and Document for Efficiency and Compliance. 

 

Presentation
Validation of Analytical Methods and Procedures

 Ludwig Huber

P-561

Design, Conduct and Document for Efficiency and Compliance.

FDA regulations and official FDA Guidelines

 

FDA Guidance
Analytical Procedures and Methods Validation

F-505 

Draft

 

FDA Guidance
Bioanalytical Method Validation

F-507

Other regulations, official guidelines and recommendations from industry task forces

 

Presentations, publications, interviews with FDA personnel (these are not official guidelines)

 

FDA Presentation
FDA Perspective on Laboratory Inspections

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.

 

FDA Presentation
Insight on FDA Inspections and Recommendations

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.

 

FDA Presentation
T. Savage, US FDA: Laboratory GMPs and Inspectional Issues:
an FDA Perspective

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.

 

FDA Presentation
Edwin Rivera: Investigating OOS Test Results for Pharmaceutical Productsl

G-334

 

FDA Presentation:
How much can you change an official method before it isn't the official method any more?

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. 

 

FDA Presentation
Analytical Methods Transfer

G-426

Kathy Lee, M.S.
Food and Drug Administration, Center for Drug Evaluation and Review, Office of Biotechnology Products, Division of Therapeutic Proteins

With three case studies

 

FDA Presentation
Analytical Methods Validation

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.

 

 

FDA Presentation
Quality by Design Approaches to Analytical Methods - FDA Perspective

G-428

Yubing Tang, Ph.D., FDA/CDER/ONDQA, AAPS, Washington DC
Shows the direction of the FDA towards Quality by Design Approaches  for analytical method validation. Most useful are the life-cycle process and examples for implementation.

 

FDA Presentation
Regulatory Perspective on Analytical Procedures and Method Validation

G-429

Alfred V. Del Grosso, Ph.D., FDA – Center for Biologics Evaluation and Research
Office of Compliance and Biologics Quality, Division of Product Quality