I work in the pharmaceutical industry. We are in the process of validating our methods. The first part of this being instrument validation. If there a concise listing of USP/FDA requirements for this. I am using a Procedure from a Laboratory managers handbook. It basically tests pump flow, detector linearity, and correlation coefficients for sample injections. Is this adequate?

Hardware tests such as pump flow, detector linearity, etc. can be useful for determining if components are operating correctly at a given point in time, but are of limited use where it counts: To be able to show that your data is accurate. To accomplish this, you need a properly validated method, which is then run with ongoing system suitability standards or interspersed control standards. These verify that the entire system is working correclty at the time your samples are analyzed. The USP has a description of system suitability. You can also find good references for method validation on the FDA website (www.fda.gov). A variety of articles have been published describing various ways to do this, see references by Huber or Pritchett.

We use the IQ/OQ/PQ approach. IQ - Installation Qualification - documents that the system (hardware and software) was installed properly. OQ - Operational Qualification - documents that each component of the system is operating within specifications. We do this by assessing critical operating parameters for each module and documenting the results. Critical parameters may be things like injection volume accuracy, reproducibility and linearity for an autosampler or temperature accuracy for a column heater. The actual tests and specifications are system dependent and need to be established by the end user. Manufacturer's specifications are a good starting point, however, these may not be accurate depending upon the age or condition of the equipment. OQ testing is repeated on a periodic, scheduled basis. PQ - Performance Qualification - documents the continued acceptable performance of the system using system suitability standards to monitor critical, method specific, parameters, such as resolution, tailing, injection reproducibility, etc.

As always, documentation is all important. You should have an IQ/OQ/PQ SOP in place for each instrument, follow it, and document the results.

Hope this helps.

Regards,

Michael Hinsberg
Hinsbar Laboratories, Inc.

http://www.hinsbarlabs.com

The International Committee on Harmonization (ICH) is a European regulatory body whose recommendations are or will be adopted by most national regulatory agencies, incl. FDA. The nice thing about ICH guidelines is that they are very specific recommendations about acceptable validation procedures.

Go to www.mcclurenet.com for free copies of ICH guidelines. Look particularly at Topic Q2B on Validation of Analytical Procedures.

Fred Klink
STM