ORPILLA, CHYRA VON LOUISE M.

15-1-95353 | Quality Control 2

VALIDATION
 Validation – Validation involves a series of activities that are taking place during the life
cycle of products and processes. It also involves careful planning of various steps in the
process and all the work should be carried out in a structured way according to
standardized working procedures.
- Process validation can be defined as documented evidence that the process, operated
within established parameters, can perform effectively and reproducibly to produce a
medicinal product meeting its predetermined specifications and quality
attributes.“(FDA 1987)
- Validation (USFDA) is defined as the establishing of documented evidence which
provides a high degree of assurance that a planned process will consistently perform
according to the intended specified outcomes.
 Importance of Validation – Validation assures great importance for – Quality
Assurance and cost reduction. Validation produces a product fit for the intended use.
Quality; Safety and Effectiveness may be designed and built into the product. Validation
is a key element in assuring the quality of the product.

The different validation techniques

1. Prospective Validation
- Prospective validation is conducted before a new product is released for distribution or,
where the revisions may affect the product's characteristics, before a product made under
a revised manufacturing process is released for distribution.
2. Concurrent validation
- Concurrent validation is a subset of prospective validation and is conducted with the
intention of ultimately distributing product manufactured during the validation study.
- Concurrent validation may be conducted on a previously validated process to confirm
that the process is validated.
3. Retrospective Validation
- Retrospective validation is the validation of a process based on accumulated historical
production, testing, control, and other information for a product already in production and
distribution.
- Retrospective validation may not be feasible if all the appropriate data was not collected,
or appropriate data was not collected in a manner which allows adequate analysis.
4. Revalidation
- As long as the process operates in a state of control and no changes have been made to
the process or output product, the process does not have to be revalidated. Whether the
process is operating in a state of control is determined by analyzing day-to-day process
control data and any finished device testing data for conformance with specifications and
for variability.
 Types of Analytical Methods
 Spectral methods
The spectral techniques measure electromagnetic radiation, which is either absorbed or
emitted by sample. For example, UV visible spectroscopy, I. R. spectroscopy, N.M.R.,
E.S.R. spectroscopy, flame photometry, flourimetry etc.
  Electro analytical methods
Electro analytical methods involve the measurement of current, voltage or resistance. For
example, potentiometric, conductometry, amperometry etc.
 Chromatographic methods
There are various advanced chromatographic techniques, which are most reliable and widely
used for estimation of multi component drugs in their formulations.
1. GLC
2. HPLC
3. HPTLC4
Principles and Instrumentation of Quality Control Equipments

1. Analytical Balance – weighing the analytical sample is often the first step of any
quantitative analytical chemical method. To use the analytical balance effectively, the
analyst must have a thorough knowledge of the construction, design, and operation of the
balance.
a. The quickest way to understand the principle of how electronic balances work, is
to first understand how they are constructed. There are two basic types of
electronic balance designs.
i. Electromagnetic balancing type
ii. Electrical resistance wire type (load cell type)
2. Autoclave – An autoclave is a device to sterilize equipment and supplies by subjecting
them to high pressure saturated steam at 121 °C or more, typically for 15-20 minutes. In
its most basic form the autoclave is a pressure cooker. Autoclaves are usually made of
steel and have various configurations for removing air prior to pressurization.
3. Steam pulsing - Air dilution by using a series of steam pulses, in which the chamber is
alternately pressurized and then depressurized to near atmospheric pressure. Vacuum
pumps - Vacuum pumps to suck air or air/steam mixtures from the chamber. Autoclave
Quality Assurance Sterilization bags/pads often have a "sterilization indicator mark" that
typically darkens when the bag/pad has been processed.
4. Autotitrator – Titrators are considered to be the perfect option used for testing of
concentration that can determine the maximum precision and productivity and find
application in the field of researching and biotechnology. These systems are also widely
appreciated for their combination of simple and dependable functioning that can be easily
instrumented and designed according to the basic routine applications.
5. Incubator – All the aquatic animals rely on the oxygen present in the water (dissolved
oxygen) to live. Aquatic microorganisms use the organic matter discharged into the water
as food source. Common natural sources of organic matter include plant decay and leaf
 fall. Bacteria will break down this organic matter using the dissolved oxygen in the water
and there by produce less complex organic substances.
6. Centrifuge – Centrifuge is applying centrifugal force to separate the useful component in
mixtures of liquids and solids or liquids and liquids. Centrifuge is mainly used to separate
solids from liquids in suspension or separate two liquids with different density and non-
homogenous liquids.
7.  Conductivity meter – Conductivity measurement is an extremely widespread and useful
method, especially for quality control purposes. Surveillance of feed water purity, control
of drinking water and process water quality, estimation of the total number of ions in a
solution or direct measurement of components in process solutions can all be performed
using conductivity measurements.
8. Disintegrator – An orally administered drug must disintegrate to attain good absorption
of its active substance. The first step toward dissolution is usually the break-up of the
tablet; a process described as disintegration. The disintegration test results in a time
necessary to disintegrate a group of tablets into small particles under standard conditions.
The disintegration test is a valuable tool in quality control environments. The test is used
for batch release and trending of lot-to-lot variations during manufacturing of tablets. 

References:
 https://www.pharmatutor.org/articles/process-validation-critical-tool-in-quality-assurance
 https://bioprocessintl.com/analytical/qa-qc/points-to-consider-in-quality-control-method-
validation-and-transfer/
 https://www.pharmatutor.org/articles/information-on-validation-important-tools-of-gmp
 https://www.edrm.net/resources/frameworks-and-standards/edrm-model/review-
guide/quality-controlvalidation/
 https://www.slideshare.net/SouravSharma21/principles-and-instrumentation-of-qc-
equipments-by-sourav-sharma
 https://www.pharmatutor.org/articles/analysis-instrumental-analytical-methods