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The FDA and other regulatory agencies require that all HPLC instruments used in Quality Control are "Qualified" by pharmaceutical companies following UPS monograph <1058>. This includes Design (DQ), Installation (IQ), Operational (OQ) and Performance Qualification (PQ). Ultimately, this is the final responsibility of the laboratory to understand, execute & comply with these regulations. Qualification proves results and that the data produced is accurate and precise.

For Design Qualification / Installation Qualification / Operational Qualification  instruments must be demonstrated to be suitably Designed, Installed and Function as designed for their intended purpose. This is the responsibility of the manufacturer and the party that installs the instrument. 

For Performance Qualification / System Suitability / Performance Verification, the data produced by the HPLC instrument must be demonstrated to be accurate and reliable at the time of their use. This is the responsibility of the user of the instrument. 

What are some Qualification Criteria of IQ/OQ v. PQ?
IQ and OQ verify the Design Specifications and Functional Specifications of an HPLC instrument and PQ Tests that verify the User Specifications and are total systems tests.
 

Operational Qualification (OQ) requires validated tests for the fitness of an HPLC instrument’s components against the intended instrument design specifications. This is typically performed by an in-house person or contract organization that performs instrument repairs/preventative maintenance. The instruments are tested and qualified according to the instruments design specs.

Example of these tests would be:

  • Autosampler volume accuracy (by weighing)
  • Pump leak-down tests
Performance Qualification (PQ) tests by the laboratory should confirm and self-document that the HPLC components are functioning properly within the entire HPLC System. This should be done after a service person (in-house or contract organization) has left the building.
A Good PQ Test should be:
  • Informative and Scientifically Valid.
  • NIST Traceable.
  • Quick and Easy to perform for technicians to reliably execute them.
  • Mostly self-documenting.
  • Universal. This will help create common performance measures making Inter-Laboratory Transfers reliable, predictable and easy.

When To Perform a PQ Test on your Instrument:
Aside from regulatory issues, it is generally accepted that a Performance Qualification of any HPLC system should be done:

  • Every 6 to 12 Months
  • After any Preventative Maintenance
  • After any Upgrades
  • After any repairs
  • After moving any instrument
  • During Method Transfer and System Troubleshooting

It is also generally accepted that a PQ should be done by laboratory technicians and not by the repair or service person since you are ultimately validating the work they did. It is important to demonstrate that the work was done properly and that the original design specifications are still being met. If not, an IQ/OQ must be done first.

PQ System and Protocol Design Objectives:
The goal of any PQ protocol should follow the previous shown IQ/OQ design plans. It should not be lost in the design of any protocol that the PQ tests should be:

  • Easy to Perform
  • Reliable

A must for any PQ protocol should involve using an HPLC column in place and using a “typical” injection sequence that the lab is already familiar with.

All PQ Protocols should include:
  • Certified, NIST-traceable Analytical Solutions
  • Easy to Use
  • A dedicated HPLC Column that gives the proper performance. It must be within defined specifications and must produce the same results even after long term storage.
  • All individual test procedures should be written and must include documentation to properly validate and prove the accuracy of the test. 

The HSQ™ Kit gives you a complete set of tests and protocols to fully and completely perform performance qualifications and performance checks of your HPLC system. Any qualified chemist or lab technician can perform these tests easily and reliably at any time.

Click HERE for PQ & HSQ for HPLC Ordering Information.
Click HERE for What is the HSQ Kit?
Click HERE for Sample Test Results Easily Performed with HSQ Kit™ for HPLC Compliance


Why you should PQ your HPLC; Comparing Two Identical HPLC Instruments & Identifying Their Differences with the HSQ™ Kit

Below is an actual report containing real data from a GMP lab that developed a stability test indicating an HPLC method for a product on one of two instruments. When the method was transferred to the other instrument, some of the peaks were not showing. The lab manager used the HSQ™ Kit standard method and determined that two identical instruments with identical hours of use were very different in performance. This lab then labeled each instrument to follow good laboratory practices. Notice the differences in system sensitivity.

Your lab can have the same advantages by measuring the performance of all your HPLC systems easily using the HSQ™ Kit.

Instrument:   Agilent 1100 LC System #9 Agilent 1100 LC System #2
Performance Characteristic: Test Conditions: Performance: Performance:
System Extra-Column Dispersion: Rs test mix extrapolated N 5 uL 3 uL
Gradient Dwell Volume: Dwell Volume: 1.20 mL 1.07 mL
  Delivery Accuracy: All circuits <5% of nominal All circuits <5% of nominal
% Injector Carryover: No Wash Vial: 0% 0%
With Wash Vial: 0% 0%
Injection Precision: 10 replicate inj. 0.07% RSD 0.07% RSD
Ret. Time Precision: 10 replicate inj. 0.21% RSD 0.06% RSD
System Sensitivity: caffeine @ 273nm normalized for column efficiency peak to peak noise @ 273 nm Sens. = 363.9 mAU/µg LOD = 0.032 µg/mL Noise = 0.04 mAU Sens. = 400.6 mAU/µg LOD = 0.058 µg/mL Noise = 0.077 mAU
Pump Flow Rate Accuracy: 0.5 mL/min 100.3% 100.0%
1.0 mL/min 100.3% 100.3%  
5.0 mL/min 99.7% 99.7%
Pump Max Press: BPR, leak check Qual: to 5,000 psi, 345 bar Qual: to 5,000 psi, 345 bar
Column Oven: oven air temp<5°C of normal Qual: 20-50°C, <5°C of normal Qual: 20-50°C, <5°C of normal

Click HERE  for Latest HSQ™ Kit Software.

 

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