A Step-by-Step Guide to Analytical Method Development and Validation

Method development and validation are essential components of drug development and chemistry, manufacturing, and controls (CMC). The goal of method development and validation is to ensure that the methods used to measure the identity, purity, potency, and stability of drugs are accurate, precise, and reliable. Analytical methods are critical tools for ensuring the quality, safety, and efficacy of pharmaceutical products in the drug development process. Analytical development services performed at Emery Pharma are outlined below.

Analytical Method Development Overview:

Analytical method development is the process of selecting and optimizing analytical methods to measure a specific attribute of a drug substance or drug product. This process involves a systematic approach to evaluating and selecting suitable methods that are sensitive, specific, and robust, and can be used to measure the target attribute within acceptable limits of accuracy and precision.

Method Validation Overview:

Method validation is the process of demonstrating that an analytical method is suitable for its intended use, and that it is capable of producing reliable and consistent results over time. The validation process involves a set of procedures and tests designed to evaluate the performance characteristics of the method.

Components of method validation include:

• Accuracy
• Precision
• Specificity
• Linearity
• Range
• Limit of detection (LOD)
• Limit of quantification (LOQ)
• Ruggedness
• Robustness

Depending on the attribute being assayed, we use state-of-the-art instrumentation such as HPLC, LC-MS, HRMS, MS/MS, GC-FID/MS, NMR, plate readers, and more.

At Emery Pharma, we follow a prescribed set of key steps per regulatory (FDA, EMA, etc.) guidance, as well as instructions from the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) for any analytical method development and validation.

Step 1: Define the Analytical Method Objectives

The first step in analytical method development and validation is to define the analytical method objectives, including the attribute to be measured, the acceptance criteria, and the intended use of the method. This step involves understanding the critical quality attributes (CQAs) of the drug product or drug substance and selecting appropriate analytical methods to measure them.

Step 2: Conduct a Literature Review

Next, a literature review is conducted to identify existing methods and establish a baseline for the method development process. At Emery Pharma, we have worked on and have existing programs on virtually all types of drug modalities, thus we have access to many validated internal methods to tap into as well.

Step 3: Develop a Method Plan

The next step is to develop a method plan that outlines the methodology, instrumentation, and experimental design for method development and validation. This includes selecting suitable reference standards and reagents and developing appropriate protocols.

Step 4: Optimize the Method

At this stage, the analytical method is optimized by adjusting parameters such as sample preparation, mobile phase composition, column chemistry, and detector settings. Our analytical chemistry team collaborates closely with clients to ensure optimal method performance.

Step 5: Validate the Method

Method validation is executed under either R&D or GLP-compliant conditions depending on the regulatory needs. Our in-house Quality Assurance team ensures compliance with 21 CFR Part 58 and hosts regulatory audits as needed.

Step 6: (Optional) Transfer the Method

For clinical trials or multi-site manufacturing, Emery Pharma supports method transfer by training analysts and managing documentation to ensure reproducibility across sites.

Step 7: Sample Analysis

We conduct sample analysis under both R&D and cGMP (21 CFR Parts 210/211) conditions. Emery Pharma is an FDA-registered and DEA-licensed facility, with the necessary infrastructure and qualified instrumentation to handle regulated studies.

Let us be a part of your success story

Emery Pharma has decades of experience in analytical method development and validation. We implement procedures that ensure drugs are manufactured to the highest quality standards—safe and effective for patient use. Contact us to discuss how we can support your next study.