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USP Verification of Comp en Dial Procedures CVG CA
USP Verification of Comp en Dial Procedures CVG CA
USP Verification of Comp en Dial Procedures CVG CA
<1058> Analytical Instrument Qualification Measurement <1225> Validation of Compendial Procedures <1226> Verification of Compendial Procedures <1010> Analytical data - interpretation and treatment Reportable value
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Raw data
Defines analytical performance characteristics (precision, accuracy, etc.) Recommends data for submissions to USP-NF Provides guidance on which analytical performance characteristics are needed based on the type of test Incorporates ICH guidelines Q2A and Q2B No guidance on verifying suitability for use
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Performance Characteristic
Category I
* Yes * * * * *
No No Yes No No No No
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21 CFR 211.194(a)(2): users of analytical methods described in USPNF are not required to validate the accuracy and reliability of these methods, but merely verify their suitability under actual conditions of use. Response to industry inquiries First draft published in PF31(2). Republished in PF32(4)
<1226> Summary
The intent of this chapter is to provide general information to laboratories on the verification of compendial procedures that are being performed for the first time to yield acceptable results utilizing the laboratories personnel, equipment, and reagents. Not intended for retroactive application to already successfully established laboratory procedures. Verification consists of assessing selected Analytical Performance Characteristics, such as those which are described in chapter <1225>, to generate appropriate, relevant data rather than repeating the validation process.
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<1226> Summary
Companion to <1225> Validation of Compendial Procedures Builds on information from <1225> Applies to drug substances, drug products, and excipients Biological tests are not included; General Chapter <111> Design and Analysis of Biological Assays and <1033> Validation of Biological Assays (in development) provides guidance for validations of these procedures
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<1226> Summary
Application: titrations, chromatographic procedures (related compounds, assay, limit tests), spectroscopic tests, etc. General tests do not typically require verification (water, heavy metals, residue on ignition, etc.)
<1226> Summary
Verification of microbiological procedures is not covered in this chapter because it is covered in other USP general chapters, <51> Antimicrobial Effectiveness <61> Microbiological Examination of Nonsterile Products: Microbial Enumeration Tests <71> Sterility Tests <1227> Validation of Microbial Recovery From Pharmacopeial Articles
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Category III
Category IV
P, L
P, LOQ
S, LOD
P, L -----
P S, LOQ S, LOQ
-------
--S S
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Verification process
There are no general Validation protocols There are no general Verification protocols
Verification
DEGREE OF VERIFICATION
Full validation
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AssayDissolve 50 mg of Sodium Chloride, accurately weighed, in water and dilute with water to 50 mL. Titrate with 0.1 N silver nitrate VS, determining the endpoint potentiometrically (see Titrimetry <541>). Each mL of 0.1 N silver nitrate is equivalent to 5.844 mg of NaCl.
Verification No Maybe No No No No No
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Identification IR, UV HPLC Purity test Loss on drying, residue on ignition, Heavy metals pH Related substances Assay Titrimetry HPLC
Validation No No Yes No No No No
Verification No No Maybe No No No No
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Identification IR, UV HPLC Purity test Loss on drying, residue on ignition, Heavy metals pH Related substances Assay Titrimetry HPLC
Verification No No No No No No No
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Identification IR, UV HPLC Purity test Loss on drying, residue on ignition, Heavy metals pH Related substances Assay Titrimetry HPLC
Validation Verification Yes Yes Yes No Yes Yes Yes No Maybe Yes No Yes No No
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Identification IR, UV HPLC Purity test Loss on drying, residue on ignition, Heavy metals pH Related substances Assay Titrimetry HPLC
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Identification HPLC Specific tests Particle in injections Uniformity Dissolution Impurities: related substances residual solvents Assay
Validation No No Yes No No No No
Verification No No Yes No No No No
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Identification HPLC Specific tests Particle in injections Uniformity Dissolution Impurities: related substances residual solvents Assay
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Identification HPLC Specific tests Particle in injections Uniformity Dissolution Impurities: related substances residual solvents Assay
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Identification HPLC Specific tests Particle in injections Uniformity Dissolution Impurities: related substances residual solvents Assay
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