Validation of Tablet Manufacturing Process in the Ethiopian Pharmaceuticals Manufacturing Factory (EPHARM)

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Date

2000-05

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Addis Ababa University

Abstract

Process validation may be defined as a systematic approach to identi fyi ng, measunng, evaluating, documenting and re-evaluating a series of critical steps III the manufacturing process that require control to ensure a reproducible final product. The approach is based on the principle that "quality is not tested into a product but rather is built into a product". It is with this principle in mind that this work has been designed and conducted. The validation study was limited to the tablet manufacturing process in the Ethiopian Pharmaceuticals Manufacturing Factory (EPHARM). Three tablet products were selected, namely, Chloroquine phosphate 250 mg, Paracetamol 500 mg and Frusemide 40 mg for the study. Chloroquine phosphate, is a highly water-soluble salt with little or no compressibility problems. Paracetamol is moderately soluble in water with a high tendency to capping. Frusemide is practically insoluble in water which may pose problems in drug release. In this study, the manufacturing facility and equipment, the raw material acquisition and testing procedures, the tablet manufacturing process, and the in-process control procedures were evaluated. Samples of the in-process materials and the fini shed products were taken and tested for compliance with quality specifications. The results of the study suggest that the proportion of fines in granulations of some of the products was excessive (chloroquine phosphate). Measurements of angle of repose indicate that the granulation bulk density, flow and surface characteristics were generally good. One-way analysis of variance (ANOY A) revealed that there was significant vari ation 111 the granulation moisture content of all of the products tested. Paracetamol tablets lacked the shiny smooth appearance expected of plain, compressed tablets. High hardness variation has been observed in some products (paracetamol, frusemide) but thickness was within the specification in all cases. Two batches of paracetamol capped and, hence, failed friability test specifications. The tablets complied with the official weight variation and content uniformity specifications, but the range need to be narrowed through the use of internal specifications. Tablets of all of the products tested disintegrated within the specified time. Dissolution rate was within the official requirements in all cases. Complete in vitro drug release (90% or more of label claim) was observed in all cases, but the optimum goal of achieving 90% drug release below 30 min was not attained particularly with frusemide and in some batches of paracetamol. Standard operating procedure (SOP) was not strictly followed during some of the unit operations. The document (batch manufacturing record) was lacking the necessary details required of such a document. For example, mixing time and mixing intensity in mixers, drying time and temperature in dryers, machine speed, compression force etc. in tablet presses were not clearly stated. No in-process control activity was observed at the granulation stage and there were no quality specifications available for the granules. Machine cleaning and maintenance procedure and documentation was lacking. Personnel training was inadequate. Generally the GMP requirements in the area of facility and equipment, personnel, process validation, documentation, etc. are not fulfilled.

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Validation of Tablet Manufacturing Process

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