1.0 OBJECTIVE
1.1 To describe a procedure for hold time study of different dosage forms at various stages of processing..
2.0 SCOPE
2.1 This SOP is applicable for hold time study of tablets, liquids manufactured
3.0 RESPONSIBILITY
3.1 Officer/Executive QA shall be responsible for preparation of a protocol and execution of studies as per approved protocol and compile the report as per results of analysis.
3.2 Officer/Executive Production shall be responsible for execution of studies as per approved protocol.
3.3 Head Production/ Designee shall be responsible for checking the protocol.
3.4 Chemist QC shall be responsible for testing of the material as per specification.
3.5 Head QC/ Designee shall be responsible for review of protocol and report.
3.6 QA Manager/ Designee shall be responsible for review of protocol and report.
3.7 Head QA shall be responsible for final approval of protocol and report.
4.0 ACCOUNTABILITY
4.1 All concerned department heads
4.2 Head QA
5.0 PROCEDURE
5.1 Hold Time can be considered as the established time period for which materials (dispensed raw materials, intermediates, and bulk dosage forms awaiting final packaging) may be held under specified conditions and will remain within the defined specifications.
5.2 Hold time studies establish the time limits for holding the materials at different stages of production to ensure that the quality of the product does not produce results outside the acceptance criteria during the hold time.
5.3 A written protocol including the following details but not limited to should be prepared prior to execution of hold time studies. The protocol and report must contain a title, document No., version, date objective, scope, responsibility, procedure, description of the material or product, sample quantities, sampling method, acceptance criteria, frequency of sampling, sampling locations, pooling of samples, storage conditions, type of container, tests to be performed and limits of results, observed values, conclusion and recommendations.
5.4 Hold time studies of different dosage forms:
5.4.1 Tablets: Hold time studies for tablet dosage form shall be performed as per the table given below:
| Processing Stage | Study Time | Environmental Conditions | Storage container |
| Binder solution (if applicable) | Initial, 2, 5, 8 hours | Temp.: 15 – 25°C
RH: NMT 60% |
SS container |
| Dried granules (if applicable) | Initial, 15th day, 30th day, 45th day | Temp.: 15 – 25°C
RH: NMT 60% |
Double poly lined HDPE container |
| Blended materials | Initial, 15th day, 30th day, 45th day | Temp.: 15 – 25°C
RH: NMT 60% |
Double poly lined HDPE container |
| Compressed tablets | Initial, 30th day, 45th day, 60th day, 90th day | Temp.: 15 – 25°C
RH: NMT 60% |
Double poly lined HDPE container |
| Coating solution (if applicable) | Initial, 12, 24, 36, 48, 60, 72 hours | Temp.: 15 – 25°C
RH: NMT 60% |
SS container |
| Coated tablets (if applicable) | Initial, 30th day, 45th day, 60th day, 90th day | Temp.: 15 – 25°C
RH: NMT 60% |
Double poly lined HDPE container |
5.4.2 Liquids: Hold time studies for liquid oral dosage form shall be performed as per the table given below:
| Processing Stage | Study Time | Environmental Conditions | Storage container |
| Bulk solution before filtration | Initial, 24, 48, 72, 84 hours | Temp.: NMT 25°C
RH: Ambient |
SS container |
| Bulk solution after filtration | Initial, 24, 48, 72, 84 hours | Temp.: NMT 25°C
RH: Ambient |
SS container |
5.4.3 Note: – If any of the in process materials crosses the stipulated time period of hold time, then they shall be dealt as per SOP of Deviation Management; SOP No.: SOP/QAD/004 and the material shall be tested as per specification before release for further processing.
Reference-: WHO TRS, No. 992, Annex 4
6.0 TRAINING
6.1 Trainer – Head-QA.
6.2 Trainee – All Concern Person.
6.3 Period – One hour or as per required.
7.0 DISTRIBUION
7.1 One set of master copy & controlled copy submitted the quality assurance department.
8.0 ENCLOSURE
8.1 NIL
9.0 ABBREVIATIONS
9.1 SOP : Standard Operating Procedure
9.2 QA : Quality assurance
9.3 QC : Quality Control
9.4 No. : Number
9.5 % : Percentage
9.6 RH : Relative Humidity
9.7 °C : Degree Centigrade
9.8 NMT : Not More Than
9.9 HDPE : High Density Poly Ethylene
9.10 SS : Stainless Steel