To provide a procedure for the Preparation, Qualification, Packing, Storage and usage of Working Standards.
I. PURPOSE :
To provide a procedure for the Preparation, Qualification, Packing, Storage and usage of Working Standards.
II. SCOPE :
The procedure is applicable to all the products manufactured and analysed
III. RESPONSIBILITY :
It is the responsibility of the Quality Control to follow the procedures for the preparation, Qualification, packing, storage and usage of the Working Standard.
IV. DOCUMENT REFERENCE :
SOPs : None
Forms : Working Standard Preparation Record
Working Standard Analysis Work book
Certificate of Analysis for Working Standard
Working Standard Label
V. PROCEDURE :
FINISHED PRODUCT WORKING STANDARD
A. DESCRIPTION
01. Working Standard shall be used in the analysis of a particular Product to compare its results with that of Working Standard for the identification of the Product and to identify the impurities and assaying of the Product.
B. PREPARATION
01. For the Pharmacopoeial product the current Pharmacopoeial Reference Standard for the particular product shall be procured. This is for the purpose of comparison with the in-house Working Standard prepared.
02. For Non- Pharmacopoeial products, the Reference- Working Standard shall be repared In-house. A sample of the Reference-Working standard prepared shall be sent for Structure Elucidation. The results are then compared against the references available in the literature for these products.
03. Take any one of the commercial manufacturing batch as a working standard having assay not less than 99.5% and qualify.
04. In case of non availability of the commercial batch having assay of 99.5%, the Working standard shall be prepared as per the pre-set procedure by re-crystallisation of Finished product or by processing a part of the pre-final stage intermediate upto the Finished product including the re-crystallisation by the same manufacturing method.
05. A procedure shall be developed for preparation of working standard.
06. A working Standard preparation Record shall be prepared as per the developed procedure to record the details of preparation.
07. The details of preparation of working standard shall be entered in the Record for Working Standard Preparation.
08. The preparation sheet shall contain the details, product name, Working standard lot number, batch number and quantity taken for preparation, standard quantity of materials to be taken, actual quantity taken, batch number, signature, operational instructions, duration, remarks, signature, provisions for recording the parameters such as temperature, pH at relevant operations.
C. EVALUATION
01. For Pharmacopoeial products, Working Standard shall be compared with Reference Standard for evaluation as per pharmacopoeial monograph..
02. For non-Pharmacopoeial products, Working Standard shall be compared with In-House Working - Reference Standard for the first evaluation and from the next evaluation it shall be evaluated against subsequent working standard.
03. A workbook for the Working Standard shall be issued by Quality Assurance department. The analysis work book shall contain details such as product name, Reference Standard lot no., date of analysis, analysis details, provision for signature of the analyst for each test.
04. A Certificate of Analysis (COA) shall be prepared for recording the analysis results. The COA shall contain the name of the product, pharmacopoeial reference standard lot number (if available), details of the tests, specifications, results, signatures of the persons involved in preparation, checking and signature of the approval authority.
05. The analytical details shall be entered in the Certificate of Analysis for the Working Standard from the workbook.
06. Prior to its first use, the working standard shall be analysed for IR and DSC tests (for the product having polymorphic identification test) as per concerned STP and the spectrum, thermogram shall be used in the analysis for the particular period.The results of all the batches analysed during a particular period shall be compared against those of the working standard for that period.
07. Inward details shall be maintained for Reference Standard (Pharmacopoeia) for recording the details of their usage and disposal (when the sample is left over).
08. In case the Reference Standard lot is changed, procure new lot and analyse the Working Standard sample with reference to the new lot.
D. PACKING DETAILS AND STORAGE
• Each Working Standard sample shall be identified with a label. For New products transferred from HRF
01. The Working –Reference standard supplied by the HRF shall be used with the same Batch number designated by the HRF for that year / the standard exhausts in single container packing. For Existing products
02. The working standard shall be packed in 12 containers, each containing sufficient quantity of the working standard to be used completely for a month.
03. A label shall be affixed with the working standard identification number of the12 containers (The identification number shall be in the form “XXWS/YY I/N, where, XX stands for the Product Code, WS for Working Standard, YY for the particular year of use, N indicates the number of containers packed, I the serial of Container used.
Eg.: BLWS/02 , 1/12
BL Stands for Bicalutamide, WS Stands for Working standard, 02 Stands for the Year 2002, 1 is the container number and 12 is the number of containers packed.
04. The standards shall be stored under conditions specified with respect to their storage.
05. The Working Standard allotted for a particular period (depending on the number of containers) shall be taken and the label shall be verified for the correct working standard identification number.
06. After completion of the analysis use it in regular use.
E. SCHEDULE
01. Working standard shall be prepared every year in the month of December or when ever required.
INTERMEDIATE WORKING STANDARD.
A. Description
02. A working Standard shall be prepared for the intermediates for which identification and chromatographic tests require standards.
03. The results of all the intermediates batches analysed during a particular period shall be compared against those of working standard for that period.
B. PREPARATION
01. Sufficient quantity of an approved batch of intermediate shall be taken as working standard.
C. EVALUATION
01. The analytical results shall be taken from batch analysis.
D. PACKING DETAILS AND STORAGE :
01. Working Standard for intermediate shall be packed in 4 containers, each containing sufficient quantity of working standard to be used completely for six months.
02. A label shall be affixed with the working standard identification number of the 4 containers (The identification number shall be in the form “WS-X I/N, where, WS stands for Working Standard, X for the Intermediate code, N for in which the material was paked and I (I=1-4) indicates the usage in the months of January to June(I=1), July to December (I=2) in that serial order for two years.
Eg.: WSPRU-I 1/02
WS Stands for Working standard, PRU-I Stands for PRU-I (Bicalutamide stage-1), 1 is the container number and 02 Stands for the material packed in 2002.
03. The samples shall be stored in a desiccator and kept in a refrigerator.
04. For the new products the first batch shall be evaluated with the standard supplied by the HRF and the first approved intermediate batch sample shall be taken for standard.
E. SCHEDULE
01. Intermediate working standards shall be prepared for once in two years.
RAWMATERIAL WORKING STANDARD.
A. DESCRIPTION
04. A working Standard shall be prepared for the raw material for which identification and chromatographic tests require standards.
05. The results of all the raw material batches analysed during a particular period shall be compared against those of working standard for that period.
B. PREPARATION
02. Sufficient quantity of an approved batch of raw material shall be taken as working standard.
C. EVALUATION
01. The analytical results shall be taken from batch analysis.
D. PACKING DETAILS AND STORAGE :
01. Working Standard for raw material shall be packed in 4 containers, each containing sufficient quantity of working standard to be used completely for six months.
02. A label shall be affixed with the working standard identification number of the 4 containers (The identification number shall be in the form “WS-X I/N, where, WS stands for Working Standard, X for the raw material, N for the particular year of use and I (I=1-4) indicates the usage in the months of January to June(I=1), July to December (I=2) in that serial order for two years.
03. The samples shall be stored in a desiccator and kept in a refrigerator.
04. For the new products the first batch shall be evaluated with the standard supplied bythe HRF and the first approved raw material sample shall be taken for standard.
E. SCHEDULE
Intermediate working standards shall be prepared for once in two years.
IMPURITY STANDARDS
A. DESCRIPTION
01. A working Standard shall be prepared for the intermediates for chromatographic
tests require standards.
02. The results of all the intermediates batches analysed during a particular period shall be compared against those of working standard for that period.
B. PREPARATION
01. Impurity standards shall be procured from HRF when ever required.
C. EVALUATION
01. The analytical results shall be provided by HRF.
E. PACKING DETAILS AND STORAGE :
01. Working Standard for impurities shall be packed in 2 containers, each containing sufficient quantity of working standard to be used completely for two years.
02. A label shall be affixed with the working standard identification number on the 2 containers .
03. The samples shall be stored in a desiccator and kept in a refrigerator.
E. SCHEDULE
01. Impurity working standards shall be prepared for once in two years.
Preparation, qualification, packing, storage, bythe hrf
