Method validations are performed in compliance with GLP and follow
Enthalpy's SOP 801, Pharmaceutical Services GLP Bioanalytical Method
Validation and Use, as well as the current FDA document, Bioanalytical
Method Validation - Guidance for Industry.
Below is a brief summary of Enthalpy's validation procedure:
• Validation activities are performed under FDA
GLP regulations.
• A validation operating procedure (VOP) is written
and authorized (by Sponsor) prior to method validation activities.
• Validation activities are performed under FDA
GLP regulations.
• The following method parameters are normally
evaluated during method validation:
- - Selectivity: the ability of the method to differentiate
and quantify each analyte in the presence of other components
in the sample
- - Intra/inter-day accuracy: accuracy is assessed
using three sets of calibration standards and quality control
samples
- - Intra-inter-day precision: precision is assessed
using three sets of calibration standards and quality control
samples
- - Recovery: the extraction efficiency of the analytical
method
- - Linearity: calibration curve linearity is assessed
- - Freeze/thaw stability: analyte stability is assessed
in matrix following six freeze/thaw cycles
- - 24-hour room-temperature stability: analyte stability
is assessed in matrix allowed to sit at room temperature for 24
hours
- - Autosampler/extract stability: analyte stability
is assessed in sample extracts
- - Long-term stability: analyte stability is evaluated
in matrix when stored at low temperature for an extended period
of time (enough time to bracket sample collection and analysis)
- - Stock-solution stability: analyte stability is
evaluated in each solvent used ultimately to make calibration
standards and quality control samples
• A draft validation report is issued within 30
days of completion of method validation activities. Note that long-term
stability and stock-solution stability experiments may need to be
included in an amendment report if the data has not been collected
by the time the rest of the validation activities have been completed.
• The final validation report is submitted within
10 business days of receiving Sponsor comments.
