Development and Validation Procedures | Pharmaceutical Analytical Development

Pharmaceutical Analytical Method Development and Validation Procedures

Analytical methods are carefully verified since they offer important data for safeguarding the health and safety of consumers. Current Good Manufacturing Practices need validation for every analytical technique used on a pharmaceutical product. Furthermore, before usage, must validate the techniques utilized to produce data supporting pharmaceutical manufacturing or regulatory filing.

Validated analytical methods help with drug characterization, quality control, and manufacturing batch records. This analytical test method validation offers a documented process that shows that the test technique is suitable for its intended purpose, contains proof of method performance, and guarantees the quality and reliability of findings.

Data Quality

A test method validation may be considered one component of a larger process of generating consistent and reliable quality data. The first essential component that provides the basis for producing quality data is processed analytical instrument qualification, a collection of recorded proof that the instruments employed in the technique function adequately for their intended purpose.

Before method validation, any equipment, software, or database must be certified using Installation, Operational, and Performance Qualifications.

Using a validated process with certified equipment guarantees that the design will provide valid data of acceptable quality. System Compatibility Tests ensure that the equipment, electronics, analytical procedures, and samples are part of an integrated test system to ensure product acceptability.

In collaboration with Quality Control, system suitability tests are performed. Check samples, which offer continuous assurance of the test’s performance, verify that the validated method will function under specified conditions. Verification, initial testing, and product-specific validation are all part of system suitability testing.

Method Development

Each year, a greater number of medicines are launched onto the market. These medicines may be completely new or a partial structural alteration of an already existing one. There is often a temporal lag between introducing a medication and its inclusion in pharmacopeias process analytical. This is owing to possible concerns in the continuing and increased use of these medicines, reports of new toxicities (leading in market removal), the development of patient resistance, and the launch of superior drugs by rivals. Under these circumstances, standards and analytical methods for these medications may not be accessible in the pharmacopeia. As a result, novel analytical techniques for such medicines must be developed.

Criteria that must fulfill for creating new drug analysis techniques

  1. Any pharmacopeia may reject the medicine or drug combination procedure analytical.
  2. A suitable analytical method for the medication may not be accessible in the literature due to patent restrictions.
  3. Analytical techniques for the medication from a formulation may be unavailable due to interference induced by formulation excipients.
  4. There are most likely no analytical techniques for detecting drug levels in body fluids.
  5. Analytical methods for medicine, when combined with other medicines, may be unavailable.
  6. Existing analytical methods may call for the use of expensive reagents and solvents. It may also require time-consuming extraction and separation processes that are either reliable or unreliable.

Guidelines and requirements

Although method validation is needed for all pharma test methods, theValidation of Analytical Procedures validation procedure varies significantly based on the regulatory authorities that regulate drug research, manufacturing, and the method’s purpose. Because government laws do not define the scientific approach to method validation, pharmaceutical firms and contract analytical testing labs depend on recommendations to satisfy the method’s compliance and scientific soundness requirements.

Non-binding recommendations that correspond to regulatory criteria and industry standards for safe pharmaceutical product development are provided by regulatory and government organizations such as the ICH or FDA and a collection of authoritative references for method validation. Here are some examples of advice papers that are available:

  • Validation of Analytical Procedures: Text and Methodology 
  • Guidance for Industry: Analytical Procedures and Methods Validation for Drugs and Biologics
  • Guidance for Industry: Bioanalytical Method Validation
    • Validation of Compendial Procedures
    • Verification of Compendial Procedures
    • Analytical Instrument Qualification.

Regulatory authorities’ guidance papers specify various characteristics or performance factors that must define throughout the method validation process. The nature of the test technique dictates the particular mix of variables to be examined throughout the validation process; assay validation parameters may vary considerably across procedures, depending on the aim of the essay or the chemical of interest.

Consequently, validation will show, via particular laboratory tests, that the method’s performance characteristics are dependable and suitable for the intended purpose. Must establish the criteria for verifying the acceptability of analytical data and the scope of the technique early in the process.

According to Validation of Analytical Procedures: 


Accuracy is the method’s ability to produce test results close to the actual value, either accepted as an authentic traditional or reference value. Using reference standards or calculating the percentage of recovery of a known added amount of analyte in a sample is frequently used to evaluate accuracy. Because the analytical method is expected to be accurate throughout its expected range of values, it Should evaluate the accuracy throughout the method’s desired range of values.


the degree of agreement between a series of measurements taken from multiple samples of the same homogeneous sample under strictly defined experimental conditions. It should represent the repeatability and reproducibility of the method. As with accuracy determination, must evaluate it across the expected range of measurements.


The ability to assess the analysis in category presence of components predicted to occur, such as contaminants, degraded products, and matrix; in the presence of large concentrations of other similar but not identical items, will detect the item in a specific technique even at low quantities. Again, determining the specificity of a procedure must be done across the expected range of values and under strictly defined conditions.

The detection limits

When determining how much of a substance is present, the lowest level of the substance that can be identified but not necessarily quantitated is the minimum amount of the substance in a model that can be seen but not necessarily quantitated. The tested substance with the lowest quantity in the sample gives a positive result above the noise.

Quantitation limit

The smallest analyte in a sample that can quantify with appropriate precision and accuracy under specific experimental circumstances is the lowest quantity of analyte in a model that can quantify with appropriate precision and accuracy. The established quantitation limit will illustrate the method’s lowest point in its range.


Linearity is the ability of an analytical method to produce test results proportional to the analyte’s concentration in the sample, either directly or through a well-defined mathematical transformation within a given range. If linearity is not possible, a non-linear model can be used. Any quantitative method must show a clear quantitative relationship between the assay measurement and the amount of material of interest in the tested sample. An analytical procedure’s range is the interval between the upper and lower analyte levels in the model. It has been demonstrated that the analytical method process analytical has adequate precision, accuracy, and linearity.

The robustness

An analytical method measures its ability to remain unaffected by minor but deliberate variations in method parameters and indicates its dependability under normal conditions.