The Korean Pharmacopoeia (KP XI), British Pharmacopoeia (BP 2013) and Japanese Pharmacopoeia contain monographs for the quality control of raw fusidate sodium and its formulations using high performance liquid chromatography (HPLC). However, the assay method for the determination of fusidate sodium ...
The Korean Pharmacopoeia (KP XI), British Pharmacopoeia (BP 2013) and Japanese Pharmacopoeia contain monographs for the quality control of raw fusidate sodium and its formulations using high performance liquid chromatography (HPLC). However, the assay method for the determination of fusidate sodium in commercial tablets is titration which is less specific than HPLC. In this study, we present an alternative HPLC method for quantitation of fusidate sodium in tablets. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2=0.9999$), while the RSDs for intra- and inter-day precision were 0.25-0.37 % and 0.11-0.60 %, respectively. Accuracies ranged from 99.46-100.85 %. Since the system suitability, intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).
The Korean Pharmacopoeia (KP XI), British Pharmacopoeia (BP 2013) and Japanese Pharmacopoeia contain monographs for the quality control of raw fusidate sodium and its formulations using high performance liquid chromatography (HPLC). However, the assay method for the determination of fusidate sodium in commercial tablets is titration which is less specific than HPLC. In this study, we present an alternative HPLC method for quantitation of fusidate sodium in tablets. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2=0.9999$), while the RSDs for intra- and inter-day precision were 0.25-0.37 % and 0.11-0.60 %, respectively. Accuracies ranged from 99.46-100.85 %. Since the system suitability, intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).
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문제 정의
For the above reasons, the objective of the present work is to develop a reliable, simple, affordable HPLC method for quantitation of fusidate sodium in tablets. Validation was conducted following the International Conference on Harmonization (ICH)13 and Korean Food and Drug Administration (KFDA) Validation Protocols.
제안 방법
Method was validated accordingly to ICH Q2 (R1) guideline with regard to linearity, precision, accuracy and robustness.
Precision (relative standard deviation, RSD %) of the method were assessed by six analyses in a day (Intra – day) and in three different days (Inter – day) of standard solutions at concentrations corresponding to 80, 100, 120 % of analysis concentration (0.8; 1.0 and 1.2 mg/mL).
The compositions of the mobile phase were investigated to determine the optimal chromatographic conditions. Recently, mixture of acetonitrile, 0.
대상 데이터
Experiments were conducted on Agilent 1100 HPLC system consisted of following components: G1379A Degasser, G1312 Binary Pump, G1313 Auto-sampler, G1316 Colcom (Column Oven) and G1314AVWD Detector (Agilent Technology, Santa Clara, USA). In intermediate precision validation, Shimadzu HPLC equipment included: DGU – 20A5R Degasser, two LC – 20 AD pumps, SIL – 20A autosampler, SPD-20A UV – Vis Detector, CBM – 20A communication bus module (Shimadzu Corporation, Kyoto, Japan) and CO-965 Column Oven (Jasco Corporation, Tokyo, Japan) was used.
In intermediate precision validation, Shimadzu HPLC equipment included: DGU – 20A5R Degasser, two LC – 20 AD pumps, SIL – 20A autosampler, SPD-20A UV – Vis Detector, CBM – 20A communication bus module (Shimadzu Corporation, Kyoto, Japan) and CO-965 Column Oven (Jasco Corporation, Tokyo, Japan) was used.
0 mg/mL sample solution. The experiments were performed in triplicate.
성능/효과
5 mL/min). In both case, except changes in retention time, the results of method were not affected: RSD % of peak area (n = 6) was not more than 0.31 %, number of theoretical plates were more than 10000 and symmetric factor was not less than 0.95 and not more than 1.05.
Results of recovery studies by standard addition method were ranged from 99.46 % to 100.85 % (Table 3). This also suggested that there was no interference from excipients in determining content of fusidate sodium in tablets.
참고문헌 (15)
Merck Research Laboratories, The Merck Index, 14th Ed., United States (2006).
A. H. Hikal, A. Shibl, and S. El-Hoofy, J. Pharm. Sci., 71(11), 1297-1298 (1982).
R. Leclercq, R. Bismuth, I. Casin, J. D. Cavallo, J. Croize, A. Felten, F. Goldstein, H. Monteil, C. Quentin-Noury, M. Reverdy, M. Vergnaud, and R. Roiron, J. Antimicrob. Chemother., 45(1), 27-29 (2000).
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