Page 95 - Application Handbook - Liquid Chromatography

Application No.L448
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Table 3 Permissible HPLC Adjustment Ranges According to USP 621
USP-Equivalent High-Speed
System Suitability Item Reference Value Condition Conditions
ShimPack VP-ODS Kinetex XB-C18
Valerophenone (when the ibuprofen retention time is 1.0) 1.4 1.3 1.2
Relative Retention 4-Isobutylacetophenone (when the valerophenone
Time retention time is 1.0) 1.2 1.2 1.2
Ibuprofen and valerophenone ≧2.5 7.05 6.17
Resolution
Valerophenone and 4-isobutylacetophenone ≧2.5 5.60 5.82
Ibuprofen ≦2.5 1.44 1.37
Symmetry Factor Valerophenone ≦2.5 1.04 1.05
4-Isobutylacetophenone ≦2.5 1.04 1.04
Retention Time ≦2.0 0.028 0.039
Ibuprofen
Relative Standard Peak Area Value ≦2.0 0.030 0.202
Deviation Valerophenone Retention Time ≦2.0 0.032 0.034
≦2.0
Peak Area Value
0.087
0.026
RSD (%) Retention Time ≦2.0 0.036 0.028
4-Isobutylacetophenone
Peak Area Value ≦2.0 0.033 0.218
n Ibuprofen Impurity Test
mAU
Impurities present in pharmaceuticals require strict 1000
management, as they can affect product quality in terms 750 Ibuprofen
of stability, functionality and effectiveness. In the impurity 500 F 4-isobutylacetophenone
1)
test specified for ibuprofen in USP NF , the content of the 250
ibuprofen decomposition product "4-isobutyl 0 A B C D E
acetophenone" is required to be less than 0.1 % of the 0.00 0.50 1.00 1.50 2.00 2.50 min
total. mAU
Fig. 2 shows the results obtained from analysis of an 7.5
Ibuprofen solution (12 mg/mL) using a UV-VIS absorbance E/0.413 %
detector (SPD-20AV), in which an expanded view of the 5.0 A/0.147 % Ibuprofen/99.344 %
chromatogram from approximately 0.5 minutes to 2 4-isobutylacetophenone/0.039 %
minutes is shown. The analytical conditions are shown in 2.5
Table 4. With the wide dynamic range of the SPD-20AV, B/0.003 % C/0.036 % D/0.016 % F/0.002 %
even the smallest peaks are clearly detected with high 0.0
resolution and high sensitivity. 0.6 0.7 0.8 0.9 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 2.0min

Table 4 Analytical Conditions Fig. 2 Chromatograms of Ibuprofen and Impurities
System : Nexera
Column : Kinetex XB-C18 (100 mm L. × 4.6 mm I.D., 2.6 µm)
Mobile Phase : A: 1%(wt / v)Chloroacetic Acid Water
(pH 3.0 adjusted with ammonium hydroxide)
B: Acetonitrile
A/B = 2/3 (v/v)
Flowrate : 2.0 mL/min
Column Temp. : 30 °C
Injection Vol. : 10 µL
Detection : SPD-20AV at 254 nm

[References]
1) U.S. Pharmacopeia 35-NF 30, 2012
· General Chapter <621>
· Official Monograph “ Ibuprofen”

First Edition: May. 2013

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