Quality control laboratory

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pharmaceutical analysis.


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Quality control::

Quality control deals with the system which accepts or rejects any activities or parameter which affects the quality of product and thus prevent quality deficiency. Quality control:

Definition of Q.C. by WHO:

“Q.C. is the part of GMP concerned with sampling, specification, and testing and with the organization, documentation and release procedure which ensure that the necessary and relevant tests are actually carried out and those materials are not released for use, nor product released for sale or supply, until their quality has been satisfactory. Q.C. is not confined to only laboratory operation but must be involved in all decisions, concerning with the quality of the product”. Definition of Q.C. by WHO

WHO guidelines for Q.C. laboratory:

Q.C. laboratory should be separated from production areas. Areas where biological, microbiological or radioisotope test methods are employed should be separated from each other. Control laboratory should be designed to suite the operations to be carried out in them. There should be adequate suitable storage space for samples, reference standards and records. WHO guidelines for Q.C. laboratory

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The design of the laboratories should take into account the suitability of construction materials, prevention of fumes, and ventilation. A separate room may be needed for instruments to protect them against electrical interference, vibration, contact with excessive moisture and other external factors. Samples of starting materials, packaging materials, intermediate products, bulk products and finished products must be taken by methods and personnel approved by Q.C. department.

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Test methods must be validated. Record must be made. No batch of product is to be released for sale or supply prior to certification by the authorized person from Q.C. dept. Sufficient sample of starting materials and product must be retained to permit future examination of the product if necessary.


Study Director’s Responsibilities 1. The Study Director has the responsibility for the overall conduct of the study and for its final report. 2. These responsibilities should include, but not be limited to, the following functions. Responsibilities:

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The Study Director should: a) Approve the study plan and any amendments to the study plan by dated signature. b) Ensure that the Quality Assurance personnel have a copy of the study plan and any amendments in a timely manner and communicate effectively with the Quality Assurance personnel as required during the conduct of the study. c) Ensure that study plans and amendments and Standard Operating Procedures(SOP s) are available to study personnel.

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d) Ensure that the procedures specified in the study plan are followed, and assess and document the impact of any deviations from the study plan on the quality and integrity of the study, and take appropriate corrective action if necessary. e) Ensure that all raw data generated are fully documented and recorded. f) Ensure that computerised systems used in the study have been validated.

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g) Sign and date the final report to indicate acceptance of responsibility for the validity of the data and to indicate the extent to which the study complies with these Principles of Good Laboratory Practice. h) Ensure that after completion (including termination) of the study, the study plan the final report, raw data and supporting material are archived.

Principle Investigator’s responsibility: :

The principle investigator will ensure that the delegated phases of the study are conducted in accordance with the applicable principles of Good Laboratory Practice(GLP). Principle Investigator’s responsibility:

Study personnel’s responsibilities :

1. All personnel involved in the conduct of the study must be knowledgeable in those parts of the principles of Good Laboratory Practice which are applicable to their involvement in the study. 2. Study personnel will have access to the study plan and appropriate Standard Operating Procedures applicable to their involvement in the study. It is their responsibility to comply with the instructions given in these documents. Any deviation from these instructions should be documented and communicated directly to the Study Director, and/or if appropriate, the Principal Investigator(s). Study personnel’s responsibilities

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3.All study personnel are responsible for recording raw data promptly and accurately and in compliance with these Principles of Good Laboratory Practice, and are responsible for the quality of their data. 4.Study personnel should exercise health precautions to minimise risk to themselves and to ensure the integrity of the study. They should communicate to the appropriate person any relevant known health or medical condition in order that they can be excluded from operations that may affect the study.

Commonly used instruments In Q.C. lab. :

Gas chromatography HPLC Capillary electrophoresis U.V. spectrophotometer I. R. spectrophotometer Analytical balance Karl fischer titrator Hot air oven Vaccum oven pH meter Dissolution test apparatus Disintegration test apparatus Polarimeter etc. Commonly used instruments In Q.C. lab.


Protocol is a system of rule about the correct way to act in formal situation . Each study shall have an approved written protocol that clearly indicates the objective and all methods for the conduct of study. PROTOCOL

  Protocol should contain the following items:-:

Title and statement of the purpose of the study Identification of the test and control articles by names, chemical number or code number. The name of the sponsor and the name and address of the testing facility at which the study is being conducted. The number, body weight range, sex, source of supply, strain, sub strain and age of the test system. The procedure for identification of the system. Protocol should contain the following items:-

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A description or identification of the diet used in study. Each dosage level expressed in milligrams per kilograms of body weight or other appropriate unit and frequency of administration. Type and frequency of test, analysis and measurements to be made. Records to be maintained. The date of approval of the protocol by the sponsor and the dated signature of the study director. Statistical method to be used.


It is an essential part of quality assurance . Clear and précised documents prevent errors that can occur due to oral communications and permit traceability. Document should be legible and error free. Some important documents are:- Site master file, Quality manual , Standard operating procedures , Manufacturing formula , Batch record , Specification etc. Documentation

Following are the essential properties of documents:-:

Documents should be prepared , reviewed and distributed with care after approval with signature and date by appropriate and authorized persons. Document contents should be clear, the title, purpose and nature of documents should be mentioned. Reproduction of documents should provide error free copies. Following are the essential properties of documents:-

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Documents should be reviewed at defined intervals or whenever considered necessary. Document revision system should provide for clear differentiation between recontent and superseded versions. Alterations to entries, if any should permit reading of original entry, should be signed and dated and the reason mentioned where appropriate.

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7. records should be made or completed at all stages of manufacture so as to ensure traceability. 8. records should be retained for at least one year after the expiry date of the finished product. 9. wherever data is maintained through electronic or photographic systems, defined procedures should be followed and accuracy of records checked.

Common data that every document should contain is shown in the format.:

Company name & title of document Identification number Issued date, effective date & review date Page number in manner of X of Y, history & reference. Prepared by, checked by & authorized by Common data that every document should contain is shown in the format.

Data generation and storage (Records):

Storage facility for records should reflect the need to preserve confidentially, integrity and logical retrieval. Thought should be given to the susceptibility of the records to damage from fire (heat), flood (humidity), electric or magnetic fields, dust, solvents etc. Purpose: The purpose of this procedure is to describe the requirements for the retention of laboratory documentation under GMP and the disposal of such documentation. Data generation and storage (Records)


It is the resposibility of laboratory staff to ensure all relevant documentation is kept for the specified timeframes and to archieve large quantities of documentation that is to be kept long term but not necessarily looked at on a regular basis. Scope

Retention and disposal of laboratory documentation:

The laboratory procedure a large quantity of documentation which must be clearly labeled stored and accounted for at all times for the duration of the documents retention period (minimum 13 year) Documents are stored in either in laboratory safes or in the numbered well boxes with detailed reference. Archiving system is predominantly manually hand recorded system for recording of documentation and can only be traced by manually looking through logbooks to find information. All analytical laboratory documentation is to be kept for a minimum of 13 years (unless otherwise stated ). If in doubt about what documentation must be retained, ask the laboratory manager or the QA manager. Documents must be disposed of by shredding or incineration. Retention and disposal of laboratory documentation


DEFINITION A sample from every batch of product made and the chemicals and components that make up a finished good are kept for a set period of time for use as reference material should be a problem with a specific product or batch. RETENTION SAMPLES


The sample shall consist of at least twice the quantity necessary for all tests required to determine its compliance with specification. The sample shall be stored in controlled room temperature expect where the product labeling or specification states otherwise. The sample shall be stored in the same primary container enclosure system in which the product is marked or shipped, or in one that has essentially the same characteristic. The sample shall be securely stored in accordance with their labels requirements and segregated from other material. The conditions in the store area must be supervised and recorded. CONDITIONS WHICH RETENTION SAMPLE MUST MEET

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The storage area shall be supervised by appointed responsible person from quality assurance. Access shall be restricted to authorized personnel only. Whenever a retention sample is required for repeated testing ,etc. It can only be released from the store following a written order approvable an authorized person, e.g. QA manager. An inventory list of stored sample sample shall be kept. Any released or discarded sample must be recorded. Samples found to comply with the specification should be kept for atleast 6 months. Those that do not should be kept for atleast 1 year, or any longer period specified in current regulations.


Retention samples are to be individually marked with ‘R/S’. Small boxes are to be held together in bundles of 4 or 5 with sticky tapes. Use standard size well boxes for all products, which can be ordered through the warehouse. Each well box is to be given a number that is unique and distinguishes it from all other well box. Must contain ‘R/S’ followed by 4 digit number. The 6 digit name is entered into “RETENTION SAMPLE REGISTER LOG” FINISHED GOODS RETENTION SAMPLE:-

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Samples are packed into shipper collected from warehouse. Once the well box if full of shippers, the front panel must have the well box number and date to be discarded. These are to be written as large and legible as possible. The ‘Date to be discarded ‘ is obtained by reviewing the “Retention Sample Register Log” and determining the longest/last expiry date. Then add one year to this date and that is the month and year for the discard date.


Any production, control, or distribution record that is required to be maintained in compliance with this part and is specifically associated with a batch of a drug product shall be retained for at least 1 year after the expiration date of the batch. RECORDS


These records shall include the following: The identity and quantity of each shipment of each lot of components, drug product containers, closures, and labeling; the name of the supplier; The supplier’s lot number(s) if known; the receiving code and the date of receipt. The name and location of the prime manufacturer, if different from the supplier, shall be listed if known. The results of any test or examination performed (including those performed derived therefrom . CLOSURE, AND LABELING RECORDS:-

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(c)An individual inventory record of each component, drug product container and closure and, for each component, a reconciliation of the use of each lot of such component. The inventory record shall contain sufficient information to allow determination of any batch or lot of drug product associated with the use of each component, drug product container and closure. (d) Documentation of the examination and review of labels and labeling for conformity with established specifications. (e) The disposition of rejected components, drug product containers, closure, and labeling.


The master manufacturing records should clearly identify: Name of product, product type, strength Ingredients to be added: name, alphanumeric code, amounts or dosage unit or percentage Amount of each ingredient for a batch Sequence of adding ingredients Equipment to be utilized designated by name and, where appropriate, by number rocessing steps with details of conditions such as time, temperature, speed In-process samples, testing, acceptance criteria Special precautions and hazardous conditions which exist and the necessary safety equipment to be used Theoretical yields and actual yields (action levels) Space for signature and date of operator/supervisor performing or checking each significant step . MASTER PRODUCTION AND CONTROL RECORDS:-


A Product in the marketable pack is classified as finished product. Practically a transportable pack, i.e. a shipper containing the salable pack (in retail) is considered the finished product. FINISHED PRODUCT RELEASE

WHO Guidelines:

Finished product should be held in quarantine until their final release, after which they should be stored as usable stock under conditions established by the manufacturer. For each batch of drug product, there should be an appropriate laboratory determinations of satisfactory conformity to its finished product specifications prior to release. Product failing to meet the established specifications or any other relevant quality criteria should be rejected. Reprocessing may be performed if feasible, but the reprocessed product should meet all specifications and other quality criteria to its acceptance and release. WHO Guidelines

SOP on Releasing of Finished Product:

SOP on releasing product should address the following points: Who is the authority to release a batch? He may be: a. “Authorised person” as per regulatory requirements, b. QA head, or c. Any other person suitably Authorised for this purpose. Before releasing the finished product at least following points should be considered: a. Completed B. P. C. R. b. Test reports of I. P. Q. C. c. Test reports of finished product / analysis. d. Deviations reports if any. e. Sterility reports along with environmental conditions reports. In case of sterile products. f. Any other reports related to the manufacturing and packaging of the batch. SOP on Releasing of Finished Product

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Part batch release is generally not acceptable practice. It can be done only under justified exceptional conditions, under deviation control system. A formal report / certificate of release may be prepared and should become the part of the B. P. C. R.

Quality Review :

Before a finished product is released for sale or distribution, the complete production and control records must be reviewed and assured satisfaction about the entire process of production and control. This is considered to be the last stage in the control process before the product moves out of the manufacturing premises Quality Review

WHO Guideline:

Production and control record should be reviewed and any failure of a batch to meet its specifications should be thoroughly investigated. The investigation should, if necessary, extend to other batches of the same product and other products that may have been associated with the specific failure. A written record of the investigation should be made and should include the conclusion and follow up action. WHO Guideline

Quality Audit:

A systematic and independent examination to determine whether quality activities and related results comply with planned arrangements and whether these arrangements are implemented effectively and are suitable to achieve objectives. “Audit" means audit of the auditee’s quality system to determine compliance with the relevant regulatory requirements Quality Audit

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Quality audit is basic control procedures to see a particular activity is going on as desired. If any deviations are observed then necessary corrective actions can be taken to bring the process to normal. Quality audit should be performed routinely. Normal frequency may be 4 to 6 months. It may also be performed on special occasions, e.g. in case of product recall or repeated rejection or when an inspection by the health authority is announced.

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Quality audit team may be formulated with people from various operational areas like Production QA / QC Validation Engineering Warehousing Personnel Audit members are selected on the basis of understanding the concept of GMP and GLP.

WHO Guideline:

It may be useful to supplement self inspection with a quality audit. A quality audit consist of an examination and assessment of all or part of quality system with specific purpose of improving it. A quality audit is usually conducted by outside or independent specialist or a team designed by management for this purpose. Such audit may also be extended to suppliers and contractors. WHO Guideline

Importance of quality audit :

To obtain unbiased management information To know factually if the company is at risk To assess individuals performance based on facts Compliance with GMP Identifies Deficiencies and faults and make quality improvement Importance of quality audit

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Investigate root cause of problem Helps to reduce cost Helps to control external activities Helps to educate and train people Helps to make supplier aware of your problem.

Over view of audit activities:

Preparing, approving and distributing the audit report Completing the audit Conducting the audit follow up Audit evidence Evaluating against audit criteria Audit findings Reviewing Audit conclusions Over view of audit activities

Batch release document:

All relevant paperwork for a particular batch, including samples of printed cartons, leaflet, shipper labels, Line Openings, Line Clearances records, etc. and collecting them together. Batch release document

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There should be written procedure for the distribution of each batch of a product to facilitate recall of the batch, if necessary. The distribution record should include at least the following data: name, address and number of the customer that the product is shipped to delivery order delivered date and number name, dosage form and strength of the product Quantity Product batch number Expiry date Special storage requirement or precautionary measures to handle the product.


c GMP for Pharmaceuticals, by Manohar A Potdar. Quality Manual, by D. H. Shah Good Manufacturing Practices for Pharmaceuticals, vol. 109 , Marcel Dekkar Inc., N. Y. www. who.int www.pharmaquality.com Reference

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