Issue link: https://www.e-digitaleditions.com/i/1302985
34 Pharmaceutical Technology Regulatory Sourcebook October 2020 P h a r mTe c h . c o m Data Integrity • 4.10.10. Applicability of Test Procedures • 4.10.20. Acceptance Criteria • 7.10. Interpretation of Requirements • 7.20. Rounding Rules • 8.70. Desiccator • 8.180. Temperatures • 8.190. Time. Before it can be applied, the analytical procedure for the monograph still needs to be interpreted, de- veloped, documented, and verified in accordance with USP <1226> (17), which states, "Users should have the appropriate experience, knowledge, and training to understand and be able to perform the compendial procedures as written. Verification should be conducted by the user such that the re- sults will provide confidence that the compendial procedure will perform suitably as intended." It also states, "The process of assessing the suitability of a compendial analytical test procedure under the conditions of actual use may or may not re- quire actual laboratory performance of each ana- lytical performance characteristic. The degree and extent of the verification process may depend on the level of training and experience of 'user'." Pharmacopoeias are complex documents that are not always well mapped out or consistent. Any working analytical procedure needs to include all the pharmacopeial elements. For example, how can an analyst interpret an instruction in a monograph such as "Dry over silica gel for 18 h" or "Dry for 3 hours at 105°" without knowing the applicable general chap- ters and their interaction with the General Notices? The relationships between the individual steps in an interpreted method for LOD, General Chapter <731>, the General Notices, and the ALCOA+ requirements are outlined in a later section. Figure 2. Tests, General Chapters and General Notices Required from the United States Pharmacopeia (USP) Methenamine Mandelate Monograph. USP 42 (01-May-2019) MONOGRAPH (Legal Standard) TESTS & METHODS REQUIRED SPECIFIC REQUIREMENTS FOR THE MONOGRAPH Identification (By Infrared spectroscopy) Assay (By Titrimetry) Impurities (By Gravimetry, Titrimetry & Visual Observation) Loss of Drying (By Gravimetry) Methenamine Mandelate Mandelic Acid Residue on Ignition Chloride and Sulfate MANDATORY GENERAL CHAPTERS BELOW <1000> INFORMATIONAL GENERAL CHAPTERS ABOVE <1000> GENERAL NOTICES OF THE PHARMACOPEIA (USP) <731> Loss on Drying <41> Balances <1251> Weighing on an Analytical Balance <197> SPECTROSCOPIC IDENTIFICATION TESTS (k) <854> MID INFRARED SPECTROSCOPY <1854> MID INFRARED SPECTROSCOPY—THEORY AND PRACTICE <1058> ANALYTICAL INSTRUMENT QUALIFICATION <541> TITRIMETRY <31> VOLUMETRIC APPARATUS <630> VISUAL COMPARISON <281> RESIDUE ON IGNITION STANDARDS & REAGENTS USP Reference Standard (RS) Volumetric Solution (VS) Silica Gel Methenamine Mandelate RS Volumetric Solutions 0.05 N silver nitrate in dehydrated alcohol 0.05 N ceric ammonium nitrate VS The General Notices and Requirements section (the General Notices) presents the basic assumptions, definitions, and default conditions for the interpretation and application of the United States Pharmacopeia (USP) and the National Formulary (NF). Requirements stated in these General Notices apply to all articles recognized in the USP and NF (the "compendia") and to all general chapters unless specifically stated otherwise. Methenamine Mandelate