Analytical Specifications, Standard Test Procedures and Worksheets – SOP  

SOP for Preparation of Specifications | SOP for Preparation of Standard Test Procedure in Pharmaceuticals |

  • SOP for Specifications, Standard Test Procedures and Worksheets covers below points :
    • Preparation of Analytical Specifications
    • Preparation of Standard Test Procedures
    • Preparation of Worksheets
    • Type of Analytical Specification, STP and Worksheet
    • Contents of Analytical Specification, STP and Worksheet
    • Numbering system for Analytical Specification, STP and Worksheet
    • Raw Material Specification format
    • Raw Material Analytical Worksheet format
    • Finished Product Specification format
    • Finished Product Analytical Worksheet format
    • In-process Testing Specification format
    • In-process Testing Analytical Worksheet format
    • Packaging Material Specification format
    • Packaging Material Analytical Worksheet format
    • General Item Specification format
    • General Item Analytical Worksheet format
1.0 OBJECTIVE :
  • This procedure describes the procedure for preparation and approval of Analytical Specifications, Standard Test Procedures and Worksheets.
2.0 SCOPE :
  • This procedure is applicable to preparation and approval of Analytical Specification, Standard Test Procedure (STP) and Worksheet of Raw materials, Blend, Uncoated Tablets, Coated Tablets, Filled Capsules, Finished Products, Packaging Materials and General Items.
3.0 RESPONSIBILITY :
  • Quality Control Chemist, Microbiologist and above
4.0 ACCOUNTABILITY:
  • Quality Control Head
5.0 PROCEDURE :

5.1 Prepare the Analytical Specifications, STP and Worksheet to assess the quality of the product by including all such tests and parameters which are necessary to control its quality and render it suitable for its end use.

5.2 The specification, STP and Worksheet are prepared for all raw materials, packaging material, In-process Testing samples such as blend, uncoated tablets, coated tablets, filled capsules, finished product and general items which should be tested before use for manufacturing and packing/ dispatch of product as per respective format (Refer point No. 7.0, Annexure).

5.3 Specification and STP of Pharmacopoeial Raw Material and Finished Product are prepared by referring pharmacopoeia.

5.4 In-house specification and STP are made by using the specification received from approved Vendor or by developing in-house procedure.

5.5 After receiving the production plan, Quality Control Department identifies the new specification for preparation.

5.6 The specification, STP and Worksheet are prepared/ revised by QC Chemist/ Officer as per requirement, checked by QC Officer/ Executive and approved by QC Head or his/ her designee.

5.7 Type of Analytical Specification/ STP/ Worksheet

  • Raw Material Specification/ STP/ Worksheet
  • Finished Product Specification/ STP/ Worksheet
  • In-process Testing Specification/ STP/ Worksheet
    • Blend Specification/ STP/ Worksheet
    • Uncoated tablets Specification/ STP/ Worksheet
    • Coated tablets Specification/ STP/ Worksheet
    • Filled capsules Specification/ STP/ Worksheet
  • Packaging Material Specification/ STP/ Worksheet
  • General item Specification/ STP/ Worksheet

5.8 Specification, STP and Worksheet contents

  • Header of the Specification, STP and Worksheet contents
    • Company logo with name and address
    • Name of Department (Quality Control Department)
    • Topic (Type of  Specification, STP and Worksheet)
    • Name of the Material/ Product
    • Specification Number/ STP Number/ Worksheet Number
    • Superseded
    • Review date
    • Page Number
  • Footer of the Specification, STP and Worksheet contents
    • A table contains Prepared by, Checked by and Approved by for signing with date, name and designation.
    • Attachment No. as mentioned in SOP.
  • The following general informations related with raw material are incorporated in first page of Raw Material Specification.
    • Name of the material
    • Category
    • Chemical Name (INN Name) International Nonproprietary Name
    • CAS No.
    • Molecular formula
    • Molecular weight
    • Structural formula
    • Pharmacopieal reference
    • Sampling procedure
    • Quantity of sample to be taken
    • Retest period
    • Test to be carried out in retesting
    • Storage condition
  • The following general informations related with finished product are incorporated in first page of Finished Product Specification.
    • Pharmaceutical dosage form
    • Composition
    • Category
    • Pharmacopieal reference
    • Quantity of sample to be taken
    • Shelf life
    • Storage condition
  • The following general informations related with In-process Testing samples are incorporated in first page of In-process testing specification – Blend/ Uncoated tablets/ Coated tablets/ Filled capsules.
    • Reference
    • Quantity of sample to be taken
  • The following general informations related with general item  are incorporated in first page of general item Specification.
    • Name of the material
    • Category
    • Chemical Name (INN Name) International Nonproprietary Name, if available
    • Molecular formula
    • Molecular weight
    • Structural formula
    • Quantity of sample to be taken
    • Storage condition
  • The following general informations related with raw material are incorporated in first page of Raw Material Analytical Worksheet.
    • Issued by
    • Material Name
    • Batch number
    • Quantity Received
    • Manufacturing Date
    • Expiry Date
    • Manufactured by
    • Supplied by
    • GRN number
    • Date of Received
    • A.R. number
    • Date of analysis completion
    • Specification number
    • Standard Test Procedure number
  • The following general informations related with finished product are incorporated in first page of Finished Product Analytical Worksheet.
    • Issued by
    • Product Name
    • Batch number
    • Batch Size
    • Manufacturing Date
    • Expiry Date
    • A.R. number
    • Date of analysis completion
    • Specification number
    • Standard Test Procedure number
  • The following general informations related with In-process Testing samples are incorporated in first page of In-process testing Analytical Worksheet – Blend/ Uncoated tablets/ Coated tablets/ Filled capsules
    • Issued by
    • Product Name
    • Batch number
    • Batch Size
    • Manufacturing Date
    • Expiry Date
    • A.R. number
    • Date of analysis  completion
    • Specification number
    • Standard Test Procedure number
  • The following general informations related with packaging material are incorporated in first page of Packaging Material Analytical Worksheet
    • Issued by
    • Material Name
    • Batch number/ Lot Number
    • Quantity Received
    • GRN number
    • Date of Received
    • A.R. number
    • Date of analysis completion
    • Specification number
    • Standard Test Procedure number
  • The following general informations related with General Items are incorporated in first page of General Item Analytical Worksheet
    • Issued by
    • Material Name
    • Batch number
    • Quantity Received
    • Manufacturing Date
    • Expiry Date
    • Manufactured by
    • Supplied by
    • Intimation number
    • Date of  Received
    • A.R. number
    • Date of analysis completion
    • Specification number
    • Standard Test Procedure number

5.9 The test to be performed for stability study is highlighted by keeping ‘*’ at the ending of the test name.

5.10 Finished Product Specification contains Shelf Life Specification (as per Pharmacopieal limit) and Release Specification which covers the stringent limit of testing parameters to improve the product quality.

5.11 All pages of Specification, STP and Worksheet are signed and authenticated by QC Chemist/ Officer as Prepared by, QC Senior Officer/ Executive as Checked by and QC Head or his/ her designee as Approved by.

5.12 Specification is reviewed by authorized person at prescribed frequency or earlier as required and identified for revision, if any.

5.13 Each new revision shall take into account the latest data, current technology used, regulatory and Pharmacopoeial requirement.

5.14 All pages of the specification, STP and Worksheet have respective page number of total page numbers e.g. If there are three pages in specification, the first page shall bear page 1 of 3, second page 2 of 3 and so on.

5.15 The numbering system for Analytical Specification, STP and Worksheet is as follows;

  • Raw Materials:
    • Raw materials are classified in to two categories.
      • Active Pharmaceutical Ingredient (API)
      • Excipients
      • Assign numbering for Raw Materials as follows;
        • RMX/YZ-PP-QQ
          • Where,    RM:     for Raw Material
          • X   :     for type of documents
          • i.e. S for Specification
            • STP for Standard Test Procedure
            • AW for Analytical Worksheet
          • Y   :      for category of raw material
            • i.e. A for  Active Pharmaceutical Ingredient (API)
            • E for Excipients
          • Z   :      for first alphabet of raw material name
          • PP :     for Serial number of respective alphabet
            • i.e. 01, 02, 03 and so on.
          • QQ:     for revision number of the document start from 00.
      • In case of introduction of new raw material, assign the number by giving continuous serial number with respective first alphabet of raw material.
  • Finished Products and In-process Testing samples:
    • Assign numbering for Finished Products and In-process Testing samples as follows;
      • AAB/XYY-ZZ
        • Where,    AA:     for type of specification/ STP/ Worksheet
          • i.e. FP for Finished Product
          • BL for Blend
          • UC for Uncoated tablets
          • CT for Coated tablets
          • FC for filled capsules
        • B   :     for type of documents
          • i.e. S for Specification
          • STP for Standard Test Procedure
          • AW for Analytical Worksheet
        • X   :      for first alphabet of the product.
          • First alphabet of the Generic name of the product. (Wherever it applicable).
        • YY :     for Serial number of respective alphabet.
          • i.e. 01, 02, 03 and so on.
        • ZZ :      for revision number of the document start from 00.
    • In case of introduction of new finished product, assign the number by giving continuous serial number with respective first alphabet of generic name of product.
  • Packaging Materials:
    • Assign numbering for Packaging Materials Common Specification of all packaging materials based on the generic name of the product as follows;
      • PMS/YZZ/PAA-BB
        • Where,  PMS:  for Packaging Material Specification
        • Y      :   for first alphabet of the product.
          • First alphabet of the Generic name of the product
        • ZZ   :  for Serial number of respective alphabet
          • i.e. 01, 02, 03 and so on.
        • P     : for Packaging materials
        • AA  : for Serial number for different packing style of the same generic product
        • BB  :   for revision number of the document start from 00.
    • Assign sub numbering for Packaging Materials Specification for different packaging materials such as alunimiun foil PVC/PVdC coated PVC film, carton, corrugated box to be used for the same product as follows;
      • PMS/YZZ/PAA-BB.CC
        • Where,  PMS:  for Packaging Material Specification
          • Y      :   for first alphabet of the product.
            • First alphabet of the Generic name of the product. (Wherever it applicable).
          • ZZ   :   for Serial number of respective alphabet
            • i.e. 01, 02, 03 and so on.
          • P     :   for Packaging materials
          • AA  :  for Serial number for different packing style of the same generic product
          • BB  :   for revision number of the document start from 00.
          • CC  :   for Code of Packaging Material
    • Assign numbering for Packaging Materials STP and worksheet, applicable for all products as follows;
      • PMXX-YY.ZZ
        • Where,  PM :  for Packaging Material
        • XX  :  for category of documents
          • i.e. STP for Standard Test Procedure
          • AW for Analytical worksheet
        • YY  :   for revision number of the specification start from 00.
        • ZZ  :   for Code of Packaging Material
    • Code for Packaging Material are mentioned below;
Packaging MaterialCode
PVC and PVdC coated PVC filmPV
Aluminium foil – PlainPA
Aluminium foil – PrintedAL
Plain Aluminium Base FoilAB
CartonCR
Inner CartonIC
Outer CartonOC
LeafletLF
Catch coverCC
ShrinkSH
Corrugated boxCB
BOPP tapBT
Strapping rollSR
HDPE bottleHB
Glass bottleGB
Poly-laminated paper – PlainPL
Poly-laminated paper –  PrintedPR

  • General Items:
    • Assign numbering for general items as follows.
      • Assign numbering for Raw Materials as follows;
        • GIX/Y/ZZ-AA
          • Where,    GI :     for General Item
          • X   :     for type of documents
            • i.e. S for Specification
            • STP for Standard Test Procedure
            • AW for Analytical Worksheet
          • Y   :      for first alphabet of the item (Material)
          • ZZ :      for Serial number of respective alphabet
            • i.e. 01, 02, 03 and so on.
          • AA:     for revision number of the specification start from 00.
    • All numbering system will be applicable to the documents which will revise after effective of SOP.

5.16 Completion of specification is indicated by “***End of document***”.

5.17 A common STP and Analytical Worksheet for all packaging materials shall be prepared.

5.18 Specification, STP and worksheet will be revised simultaneously and reason for revision shall be mentioned in History sheet as per annexure No.: 17

5.19 In case of Packaging Material, History sheet of specification and History sheet of STP/ Worksheet will be made separately.

5.20 Whenever required, Specification and STP will be issued to the analyst/ section head for analysis purpose.

5.21 Authorized person of documentation section-QC shall issue the specification and STP as per requirement of respective section and enter the details in specification issuance log book Annexure No.: 18

5.22 After receiving the request for Analytical Worksheet from respective section, authorized person of documentation section shall take the photocopies on white coloured A4 size paper from Original Authenticated Analytical Worksheet.

5.23 Authorized person shall authorize the photo copy of worksheet by signing as issued by with date.

5.24 Product Name and Batch No. shall be entered in worksheet by documentation section.

5.25 The details of the issuance shall be entered in analytical worksheet issuance log book Annexure No.: 19 and hand over to respective section head.

5.26 Section head shall handover worksheet with sample to the analyst.

5.27 If any discrepancy happens for the first issuance copy, the analyst shall request for a new copy with proper justification to section head in Annexure No.: 20

5.28 Section head will arrange to issue a new photo copy after verifying justification of the analyst and after taking approval from QC Head and first issuance copy will be destroyed by cutting into small pieces.

5.29 Use ‘Arial’ font with size 10 for preparation of all attached annexure.

6.0 Abbreviations:
AbbreviationExpanded form
QCQuality Control
STPStandard Test Procedure
NO.Number
INNInternational Nonproprietary Name
CAS No.Chemical Abstract Service
SOPStandard Operating Procedure
A.R.Analytical Report
BOPPBiaxially Oriented Polypropylene 
HDPEHigh Density Poly Ethylene
PVCPoly vinyl Chloride
PVdCPoly vinylidene Chloride

7.0 Annexures:
Annex. No.                           Title
01List of Raw material Specification (API/ Excipients)
02List of In-Process Specification (Blend/ Uncoated tablets/ Coated Tablets/ Filled capsules)
03List of Finished Product Specification (Impulse Products/  Loan License Products)
04List of Packaging material Specification (Impulse Products/  Loan License Products)
05Raw Material Specification
06Raw Material Standard Test Procedure
07Raw Material Analytical Worksheet
08Finished Product Specification
09Finished Product Standard Test Procedure
10Finished Product Analytical Worksheet
11In-process Testing Specification
12In-process Testing Standard Test Procedure
13In-process Testing Analytical Worksheet
14Packaging Material Specification
15Packaging Material Standard Test Procedure
16Packaging Material Analytical Worksheet
17History Sheet
18Specification/ STP Issuance Log Book
19Analytical Worksheet  Issuance Log Book
20Justification for re-issuance of analytical worksheet
21List of General Item Specification
22General Item  Specification
23General Item  Standard Test Procedure
24General Item Analytical Worksheet

8.0 SOP References:
  • Orange Guideline MHRA – Rules and Guidance for Pharmaceutical Manufacturers and Distributors – 2017, Section-2, Part-I (DOCUMENTATION)
  • Schedule L1, Drugs & Cosmetics (Third Amendment) Rules, 2008

END OF THE SOP


ANNEXURES :

Annex. No. 01 List of Raw material Specification (API/ Excipients)


Annex. No. 02 List of In-Process Specification (Blend/ Uncoated tablets/ Coated Tablets/ Filled capsules)


Annex. No. 03 List of Finished Product Specification


Annex. No. 04 List of Packaging material Specification


Annex. No. 05 Raw Material Specification


Annex. No. 06 Raw Material Standard Test Procedure


Annex. No. 07 Raw Material Analytical Worksheet


Annex. No. 08 Finished Product Specification


Annex. No. 09 Finished Product Standard Test Procedure


Annex. No. 10 Finished Product Analytical Worksheet


Annex. No. 11 In-process Testing Specification


Annex. No. 12 In-process Testing Standard Test Procedure


Annex. No. 13 In-process Testing Analytical Worksheet


Annex. No. 14 Packaging Material Specification


Annex. No. 15 Packaging Material Standard Test Procedure


Annex. No. 16 Packaging Material Analytical Worksheet


Annex. No. 17 History Sheet


Annex. No. 18 Specification/ STP Issuance Log Book


Annex. No. 19 Analytical Worksheet Issuance Log Book


Annex. No. 20 Justification for re-issuance of analytical worksheet


Annex. No. 21 List of General Item Specification


Annex. No. 22 General Item Specification


Annex. No. 23 General Item Standard Test Procedure


Annex. No. 24 General Item Analytical Worksheet