Preparation, Approval and Control of Specifications and Standard Test Procedures
Objective
To lay down a procedure for the preparation, approval and control of Specifications and Standard Test Procedures for raw materials, packaging materials, in-process materials and finished products.
Scope
This Standard Operating Procedure is applicable for the preparation and implementation of all Specifications and Standard Test Procedures.
Responsibility
Scientist, Documentation Cell (R&D) to prepare Specifications and STPs for raw materials, in-process materials and finished products in coordination with Scientist, Formulation Research and Development and Scientist, Analytical Research and Development respectively.
Scientist, Packaging Development, to prepare Specifications and STPs for packaging materials. Scientist In-charge or Group Leader, Packaging Development shall check the Specifications and STPs.
Group Leader, Analytical Research & Development to check the STPs and Specifications for the materials other than packaging materials.
Head, Analytical Research & Development or his/her designee and Head, Quality Control or his/her designee to approve Standard Test Procedures and Specifications.
Head, Formulation Research or his/her designee and to approve Specifications and STPs.
Head, Regulatory Affairs or his/her designee to approve Specifications and STPs.
Head, Quality Assurance or his/her designee shall be responsible for final approval of Specifications and Standard Test Procedures.
Abbreviations and Definitions
Specifications : A controlled document which describes a set of physical, chemical, biological or microbiological requirements that a product or material must meet. These are expressed numerically, in general or where applicable, in terms of appropriate units together with their limits, and are designed to measure the quality of the material.
The Specifications that determine whether a drug product is suitable for release at the time of its manufacture are known as ‘Release Specifications’ and the Specifications that must meet up to its retest date, in case of active ingredient or its shelf life, in case of drug product are known as ‘Shelf Life Specifications’. The specifications applied for stability studies shall be termed as ‘Stability Specifications’.
STP : Standard Test Procedure; a controlled document which describes a detailed instructions (laid as per specifications designed for a product or material) to be followed to analyze or assess the material for its quality.
GTP : General Test Procedure; a controlled document which shall define general test methodologies for testing of materials. The GTPs shall be prepared as per SOP titled ‘Preparation, Approval and Control of General Test Procedures’.
Procedure
Preparation and Approval of Specifications and STPs
All Specifications and STPs shall be written in clear and easy to understand language.
All specifications and STPs shall be printed on one side of standard A-4 size white paper of appropriate quality in black ink.
All Specifications/ STPs shall be prepared using Microsoft Word application software
Page setup and Page border settings.
Top margin shall be 0.8 inch (0.8”)
Bottom margin shall be 0.6 inch (0.6”)
Left margins shall be 0.6 inch (0.6”)
Right margin shall be 0.6 inch (0.6”)
All Specifications and STPs shall be generated on computer in the formats respectively given in Annexure-1 (Specifications) and Annexure-2 (Standard Test Procedure) and shall be typed in font face ‘Times New Roman’ with font size ‘12’ or with other appropriate font size.
Company corporate logo shall be printed on the top left hand side of the standard “A4” sheets of good quality.
Word ‘Specifications’ in case of Specifications and words ‘Standard Test Procedure’ in case of STP shall be typed in bold on the top middle position of the page (font size 13).
Word ‘Type:’ shall be in bold on the top right side of the page (font size 13). Under this column, type of Specifications/ STP shall be mentioned as given below
For the Specifications/STP belonging to a raw material, ‘Raw Material’ shall be typed in regular text.
For the Specifications/STP belonging to a packaging material, ‘Packaging Material’ shall be typed in regular text.
For the Specifications/STP belonging to In-process material, ‘In-process’ suffixed with S1, S2, S3…..shall be typed in regular text e.g. for Specifications of granules for tablets which is first stage in-process material of tablets, ‘In-process-S1’shall be typed.
For the Specifications/STP belonging to Finished Product, ‘Finished Product-Release’ shall be typed if specifications are Release Specifications. Similarly for Shelf Life Specifications and Stability Specifications, ‘Finished Product-Shelf Life’ and Finished Product-Stability’ shall be typed respectively, in regular text.
‘Title’ of the Specifications/ STPs shall be brief and self descriptive in nature. It shall be typed in regular text keeping the first letter of the key words in capitals (i.e. title case).
‘Reference’ shall be clearly mentioned in this column as pharmacopoeial or in-house. In case of pharmacopoeial reference mention BP/IP/Ph.Eur./USP/USNF, etc. as applicable and in case of in-house reference write IH or In-house in regular text.
‘Item Code’ of the material shall be mentioned here (refer SOPs titled ‘Assigning Item codes to Raw Materials, Packaging Materials, In-process Materials and Finished Products’) in regular text.
‘Page No.’ shall be numbered, as specific page number of the total pages of Specifications/ STPs e.g. first page of Specifications of total 03 pages shall be 01 of 03.
‘Specification No.’ and ‘STP No.’ shall be an alphanumeric number.
Specification Number and STP Number for Raw Materials: The specification number for raw material shall be denoted as ‘Item Code-S’ along with its Revision Number as ‘Rev. No. XX’. STP number for raw material shall be denoted as ‘Item Code-T’ along with its Revision Number as ‘Rev. No. XX’. where,
Item code: an alphanumeric code assigned for the raw material as per SOP ‘Assigning Item codes to Raw Materials, Packaging Materials, In-process Materials and Finished Products’).
– : dash
S or T : S denotes Specifications, in case of Specification No. and T denotes Test procedure, in case of
STP No.
XX : denotes the revision number which shall be of two numeric characters starting from 00 in case of first version of Specifications or STP.
e.g. The first version of Specifications for raw material with item code AAA018 shall be written as AAA018-S Rev. No. 00 under the column ‘Specification No.’ and its first revision shall be given as AAA018-S Rev.No.01 under the column ‘Specification No.’ of the Specifications. Similarly, the first version of an STP for raw material with item code AAA018 shall be written as AAA018-T Rev.No.00 under the column ‘STP No.’ in case of STP and STP number shall be written as AAA018-T (not with its revision number) under the column ‘Reference Test Method’ in case of Specifications.
Specification Number and STP number for Packaging Material: The specification number for packaging material shall be denoted as ‘Item Code-S’ along with its Revision Number as ‘Rev. No. XX’ and ‘Item Code-T’ with its Revision Number as ‘Rev. No. XX’ respectively where,
Item code: an alphanumeric code assigned for the packaging material as per SOP ‘Assigning Item codes to Raw Materials, Packaging Materials, In-process Materials and Finished Products’).
– : dash
S or T : S denotes Specifications, in case of Specification No. and T denotes Test procedure, in case of
STP No
XX : denotes the revision number which shall be of two numeric characters starting from 00 in case of first version of Specifications or STP. e.g. second revision of Specifications for packaging material with item code BBB039 shall be written as BBB039-S Rev. No. 02 under the column ‘Specification No.’ In case of STP for this packaging material, STP No. shall be mentioned as BBB039-T Rev. No. 01 if it is the first revision of this STP. Under the ‘Reference Test Method’ column in Specifications/ STP No. shall be mentioned as BBB039-T (not with its revision number)
In case the same packaging component with item code BBB039 is redesigned or modified, the revised item shall be given item code as BBB039A (refer SOP titled ‘Assigning Item codes to Raw Materials, Packaging Materials, In-process Materials and Finished Products’) and the relevant Specifications with specification number BBB039-S Rev. No. 02 shall be revised to give specification number BBB039A-S Rev. No. 03 under ‘Specification No.’ column and BBB039-S Rev. No. 02 under ‘Supersedes’ column of the Specifications.
Note: In case of GTPs for testing of packaging materials, the same shall be prepared and numbered as per SOP titled ‘Preparation, Approval and Control of General Test Procedures’).
The Specification Number and STP Number for In-process Material: Specification Number and STP Number shall be denoted as ‘Item Code-S’ along with Revision Number as ‘Rev. No. XX’ and ‘Item Code-T’ along with Revision Number as ‘Rev. No. XX’ respectively, where
Item code : an alphanumeric code assigned for the In-process material as per SOP ‘Assigning Item codes to Raw Materials, Packaging Materials, In-process Materials and Finished Products’
– : dash
S or T : S denotes Specifications, in case of specification No. and T denotes Test procedure, in case of STP No.
XX : denotes the revision number which shall be of two numeric characters starting from 00 in case of first version of Specifications or STP
e.g. Specification number for the first version of Specifications of In-process material with item code S2038 shall be written as S2038-S Rev.No.00 under column ‘Specification No.’ and S2038-T Rev.No.00 shall be written as STP number for the first version of STP for the in-process material with same item code.
Specification Number and STP Number for Finished Products: The specification number/STP number of finished products shall be denoted as ‘Finished Product Code-CC’ along with Revision Number as ‘Rev. No. XX’ and ‘Finished Product Code-CC’ along with Revision Number as ‘Rev. No. XX’ respectively, where
Finished Product code: an alphanumeric code assigned for the Finished Product as per SOP ‘Assigning Item codes to Raw Materials, Packaging Materials, In-process Materials and Finished Products’.
– : dash
S or T : S denotes Specifications, in case of specification No. and T denotes Test procedure, in case of STP No.
Y : shall represent the following:
‘R’, in case of Release Specifications/ STP
‘L’, in case of Shelf Life Specifications/STP
‘S’, in case of Stability Specifications/STP
XX : denotes the revision number which shall be of two numeric characters starting from 00 in case of first version of Specifications or STP
e.g. Specification number for the first version of Release Specifications of Finished Product with code F038ST1200 shall be written as F038ST1200-SR Rev.No.00 under column ‘Specification No.’ and F038ST1200-TR Rev.No.00 shall be written as STP number for the first version of STP for the finished product with same finished product code.
‘Supersedes’: Superseded number of the Specifications/STP shall be given in this column. For example, In case of Finished product Release Specifications of tablets the specification number is F038ST1200-SR Rev.No.00 when prepared for the first time (first version), ‘Supersedes’ column shall be filled with the word ‘None’ and when the same is revised for the first time, ‘Supersedes’ shall be given as F038ST1200-SR Rev.No.00 and under ‘Specification No.’ F038ST1200-SR Rev.No.01 shall be mentioned.
‘Reference Test Method’: Reference test method shall be the method adopted for testing of material ; for example a Raw material with item code ‘DDD012’ then DDD012-T denotes the reference test method for that particular raw material.
‘Effective Date’ is the date when the contents of Specifications/ STPs become operational for the user department(s). It shall be given after approval of proposed Specifications/ STPs by QA department in DD-MM-YY format, by hand.
The ‘Next Review Date’ shall be two years from the Effective Date of the Specifications/ STPs, given by QA department in DD-MM-YY format, by hand. Every Specifications/ STP shall be revised within two months of Next Review Date or earlier, if any amendment is required (refer point number 5.2. for more details).
‘Reference’ shall be clearly mentioned in this column as pharmacopoeial or in-house. In case of pharmacopoeial reference mention BP/IP/Ph.Eur./USP/USNF, etc. as applicable and in case of in-house reference write IH or In-house in regular text.
The concerned Scientist and Scientist In-charge or Group Leader shall sign in the column ‘Prepared by’ and ‘Checked by’ respectively.
In case of STPs, Head, Analytical Research & Development or his/ her designee and Head, Quality Control or his/ her designee shall sign in the column ‘Approved by’ under R&D and QC heads respectively.
In case of Specifications, Head, Formulation Research or his/ her designee and Head, Quality Control or his/ her designee shall sign in the column ‘Approved by’ under R&D and QC heads respectively.
Head, QA or his / her designee shall approve the Specifications and STP by signing the same in the column ‘Approved by’ under QA head
Note: Heading entries as described in Annexure-1 and Annexure-2 shall be typed in bold with font size of 12. All the entries made in hand by the concerned personnel shall be in black ink. Ink of good quality shall be used for the purpose.
Different steps of STP shall be typed using outline numbering system.
The tests, which shall be performed during retesting of materials, shall be indicated by ‘*’ (asterisk) in the Specifications.
Depending upon the type of material, the Specifications can also be mentioned with the other information related to handling precautions, storage/packaging, indication on periodic (skip) tests (tests which are not always conducted on a batch-by-batch basis), frequency of retesting, reference of sampling procedure, name of approved vendor and any other requirement like in case of certain raw material specifications, requirement for extra test reports from the vendor, can be given.
An STP may carry the reference of GTPs for certain tests. These GTPs as a part of STP shall be followed to analyze the material.
Review and Control of Specifications/STPs
A history sheet shall be generated and maintained by R&D for each STP/ Specification as per Annexure-3.
Preparation of Master copies and Controlled copies, distribution and retrieval, review and/ or revision of Specifications and STPs shall be undertaken as per SOP titled ‘Document and Data Control’
All Specifications/ STPs shall be reviewed biennially i.e. once in two years. QA shall identify the Specifications/ STPs at least two months before approaching the end of two years from the effective date. QA shall initiate review process as per SOP titled ‘Document and Data Control’
Forms and Records
Annexure-1 : Specimen Format of Specifications
Annexure-2 : Specimen Format of Standard Test Procedure
Annexure-3 : History Sheet ( Specification /STP)
Distribution
Master Copy – Documentation Cell (Quality Assurance)
Controlled Copies – Analytical Research & Development (R&D),Documentation Cell (R&D), Packaging Development (R&D), Quality Control
- History
| Date | Revision Number |
Reason for Revision |
| 00 | New SOPs |
Annexure-1
Specimen Format of Specifications
Annexure-2
Specimen Format of Standard Test Procedure
Annexure-3
History Sheet ( Specification /STP)