Pharmacopeias procedures

A.ccording to Slowick and Kelley , the U. S. Pharmacopeia procedure, when carried out as directed, is slow, requiring about 9 hours, and their findings show that it tends to give somewhat high results wth variations of... 

Sterility testing is conducted on each lot of ophthalmic product by suitable procedures, as set forth in the appropriate pharmacopeia and validated in each manufacturer s laboratory. While the majority of ophthalmic preparations contain preservatives for multiple-dose use, sterile preparations in special containers for individual use on a single patient must be made available. This availability is especially critical for every hospital, office, or other installation where accidentally or surgically traumatized eyes are treated, as well as for patients intolerant to preservatives. 

The use of concordant methods does not necessarily require identical reagents, procedures, or measurements. Official procedures of pharmacopeias per se require no validation, but validation of the applicability of such to each preparation (formulation) is to be presumed (e.g., the presence of interfering ingredients). 

Coenegracht et al. [3] have introduced a four solvent system to compose mobile phases for the separation of the parent alkaloids in different medicinal dry plant materials, like Cinchona bark and Opium. Through the use of mixture designs and response surface modeling an optimal mobile phase was found for each type of plant material. These new mobile phases resulted in equally good or better separations than obtained by the procedures of the Pharmacopeias. Although separations were as predicted, the accuracy of the quantitative predictions needed to be improved. 

Reproducibility Reproducibility measures the precision between laboratories. This parameter is considered in the standardization of an analytical procedure (e.g., inclusion of procedures in pharmacopeias and method transfer between different laboratories). 

U.S. Pharmacopeia (USP), General Chapter (1225), Validation of compendial procedures, USP, Rockville, MD. 

The basic sterilization procedures involve the application of dry or moist heat, the use of sterilizing radiation or, more recently, the use of intense bright light. A valuable source of information is the section on Sterilization and Sterility Assurance of Compendial Articles in the General Information Chapter (<1211>) of the United States Pharmacopeia, now in its 28th revision. Since it is now revised on an annual basis the interested reader is referred to the latest edition for up-to-date information. 

Harmonization may be carried out retrospectively for existing monographs or chapters or prospectively for new monographs or chapters. The three pharmacopeias have a commitment to respect the agreed working procedures and the associated time deadlines as an essential part of the harmonization procedure. The PDG has defined harmonization of a pharmacopeial monograph or general chapter as follows ... 

When using a fully harmonized pharmacopeial monograph or general chapter, an analyst will perform the same procedures and reach the same accept/reject decisions irrespective of which PDG pharmacopeia is referenced. This approach is called interchangeability, and each pharmacopeia will identify, in an appropriate manner, such a monograph or general chapter. 

For a subject to be harmonized retrospectively, the coordinating pharmacopeia collects the information on the existing specifications in the three pharmacopeias, on the grades of products marketed, and on the potential analytical procedures. 

Stage 2 ends with the proposal draft, which is mentioned in this procedure as a Stage 3 draft. The Stage 3 draft, accompanied by supporting comments or data that explain the reasons for each test procedure or limit proposed, is sent by the coordinating pharmacopeia to the secretariats of the other two PDG pharmacopeias. 

The corresponding secretariats may have to add information essential to the understanding of the implementation of the texts (e.g., the description of an analytical procedure or of reagents that do not exist in the pharmacopeia) and a translation is added by the European and Japanese Pharmacopoeias. The style may be adapted to that of the pharmacopeia concerned or global style may be used. A pharmacopeia can add text, either to amplify some of the requirements with additional information or because national requirements and compendial policy dictate that the addition is necessary. However, there must be a clear indication that this additional information is not part of the harmonized document. This will avoid additional text being included after the harmonization process is completed, but will allow interested parties to review a complete text. The three pharmacopeias endeavor to publish the drafts simultaneously or as close together as possible. 

The document is submitted for adoption to the organization responsible for each pharmacopeia. Each pharmacopeia incorporates the harmonized draft according to its own procedures. Stylistic and editorial differences may occur. 

Analytical reagents used in testing the excipients should be prepared and labeled following established procedures. Retest or expiration dates should be used, as appropriate, for analytical reagents, or standard solutions. Analytical methods should be validated unless the method employed is set forth in the current revision of the United States Pharmacopeia/National Formulary, Association of Official Analytical Chemists (AOAC), Book of Methods, or other recognized standard references, or detailed in the Drug Master File or approved New Drug Application and are used unmodified. 

A regulatory analytical procedure is the analytical procedure used to evaluate a defined characteristic of the drug substance or drug product. The analytical procedures in the U.S. Pharmacopeia/National Formulary (USP/NF) are those legally recognized under section 501(b) of the Act as the regulatory analytical procedures for compendial items. 

Specifications used by quality control to release drug A are found in a laboratory procedure. In addition to the previously discussed hardness and disintegration time requirements, the procedure calls for determining the average tablet weight by the United States Pharmacopeia (USP) procedure that is, 20 individual tablets are weighed. 

Assessment of indomethacin powder had been specified in the U.J5. XIX and the British Pharmacopeia, 1980 as a back titration with hydrochloric acid after alkaline hydrolysis(13,14). This method can attain a precision of + 0.8%(62). A direct titration for tablets and capsules is described using sodium hydroxide. If performed rapidly with phenolphthalein indicator, a precision of +0.3% is attainable. 8 The latter procedure serves to differentiate ester formation as well as hydrolysis products from intact material. The presence of parachlorobenzoic acid and 5-methoxy-2-methylindole-3-acetic acid are cause for positive error. 

Failure to establish yields or acceptable levels of rejects for both in-process and finished product Failure to conduct stability studies Manufacturing equipment not identified and/or qualified Inadequate training of employees working in aseptic operations Inadequate process change procedures Validation protocols that lack acceptance criteria Incomplete investigations of laboratory failures Failure to follow United States Pharmacopeia (USP) procedures for the bacterial endotoxin test... 

The United States Pharmacopeia-National Formulary (USP-NF), USP34-NF29 SI. General InformationM 1225>Validation of Compendial Procedures, pp 779-782. Pharmacopeial Forum 35(2) 444... 

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