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 Material	Code
PVC and PVdC coated PVC film	PV
Aluminium foil – Plain	PA
Aluminium foil – Printed	AL
Plain Aluminium Base Foil	AB
Carton	CR
Inner Carton	IC
Outer Carton	OC
Leaflet	LF
Catch cover	CC
Shrink	SH
Corrugated box	CB
BOPP tap	BT
Strapping roll	SR
HDPE bottle	HB
Glass bottle	GB
Poly-laminated paper – Plain	PL
Poly-laminated paper – Printed	PR

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:

Abbreviation	Expanded form
QC	Quality Control
STP	Standard Test Procedure
NO.	Number
INN	International Nonproprietary Name
CAS No.	Chemical Abstract Service
SOP	Standard Operating Procedure
A.R.	Analytical Report
BOPP	Biaxially Oriented Polypropylene
HDPE	High Density Poly Ethylene
PVC	Poly vinyl Chloride
PVdC	Poly vinylidene Chloride

7.0 Annexures:

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