5989_9241en.qxd

Development and validation of an
HPLC method to analyze ibuprofen and
impurities according to the European
Pharmacopoeia
Abstract
This Application Note describes the development of a fast, accurate, and reproducible method to analyze ibuprofen and related impurities according to European Pharmacopoeia (EP) regulations1, using an Agilent 1120 Compact LC. The experiments described in this Application Note include determination of precision of areas and reten- tion times, as well as chromatographic parameters like resolution and signal-to-noise ratios. The experiments prove precise results from a system that was optimized for everyday productivity, and they fulfill Introduction
Step 1 – Preparation of individual Step 2 – Preparation of solution Step 3 – Preparation of reference tion from step 2 was added andthe mixture was diluted to 10 mL (6 µg/mL) of each of the impurities.
Experimental
Chromatographic conditions
System suitability and performance
Equipment
Preparation of samples
Solvents, gradient, and pump settings
main peak must be linear with-out dilution.
Number of injections
Verify baseline stability and identify artifacts Verify stability of response and correctness of Results and discussion
Table 1
Setup for testing system suitability and performance.
Retention time (min)
Resolution
ria were fulfilled. The requiredsensitivity was obtained for all Table 2
Results for control sample: resolution and signal-to-noise (S/N) ratio.
peaks and resolution > 1.5 wasachieved for all compounds in the Compound
Retention time (min)
(µg/mL)
Suitability sample: precision of retention times and areas. (RSD = relative standard deviation; RT
= retention time).
was proven. For all components,the criteria for precision of reten- Residual r
standard deviation
tion times and areas were fulfilled,showing that the system can be Calibration (Setting “Ignore Origin”, y=mx+b, 0.6 to 9 µg/mL for impurities and 0.2 to 3 mg/L for
ibuprofen).
the concentration of the referencesolution) to the highest concentra- References
correlation results (r>0.999) dur-ing calibration, which is also proof European Pharmacopoeia 4.2,
Council of Europe, 2737-9, 2002.
Conclusion
Specifications, Ordering,” Agilent 5989-7454ENA, 2008.
use, as well as the lowest cost-of-ownership for standard LC Substances, Revision 2,http://www.fda.gov/cder/guid- ance/7838fnl.pdf, 2008.
from a system that was optimizedfor everyday productivity, and to number 5989-5621EN, 2006.
results show that the instrument iswithin the limits of the regulatoryrequirements for a quality controlenvironment.
The results show explicitly theapplicability of the 1120 LC sys-tem for pharmaceutical testing in QA/QC departments. In additionto the instrument capabilities, the new version of the Agilent wide range of features for dataanalysis and reporting of theresults.
www.agilent.com/chem/1120
Published June 15, 2010Publication Number 5989-9241EN

Source: http://anatox.de/Datenblaetter_Publikationen/5989-9241EN.pdf