HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.
ANALYTICAL METHOD VALIDATION
10 and 20mg Fluoxetine Capsules HPLC Determination
FLUOXETINE HCl
C17H18F3NO•HCl
M.W. = 345.79
CAS — 59333-67-4
tidSTABILITY INDICATING
A S S A Y V A L I D A T I O N
Method is suitable for:
tem4成绩查询ýIn-process control
þProduct Relea
þStability indicating analysis (Suitability - US/EU Product) CAUTION
FLUOXETINE HYDROCHLORIDE IS A HAZARDOUS CHEMICAL AND SHOULD BE HANDLED ONLY UNDER CONDITIONS SUITABLE FOR HAZARDOUS WORK.
IT IS HIGHLY PRESSURE SENSITIVE AND ADEQUATE PRECAUTIONS SHOULD BE TAKEN TO AVOID ANY MECHANICAL FORCE (SUCH AS GRINDING, CRUSHING, ETC.) ON THE POWDER.
ED. N0: 04Effective Date:APPROVED::
HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.
ANALYTICAL METHOD VALIDATION
10 and 20mg Fluoxetine Capsules HPLC Determination
TABLE OF System Repeatability ................................................................................................................ Intermediate Precision .............................................................................................................. . Accuracy of Accuracy of the . VALIDATION OF FLUOXETINE HCl AT Linearity at Accuracy of Fluoxetine HCl at VALIDA
TION FOR META-FLUOXETINE HCl (POSSIBLE IMPURITIES).................................. Meta-Fluoxetine HCl linearity at 0.05% - 1.0%........................................................................... Detection Limit for Quantitation Limit for Meta Accuracy for Meta-Fluoxetine HCl ............................................................................................ Method Repeatability for Intermediate Precision for SPECIFICITY - STABILITY INDICATING EVALUATION OF FORCED DEGRADATION OF FINISHED PRODUCT
1.
2. Acid Hydrolysis
3. Ba hydrolysis
4. Oxidation
5. Sunlight
6. Heat of solution
纬度英语7. Heat of powder System Suitability STABILITY OF STANDARD AND .
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HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.
ANALYTICAL METHOD VALIDATION
10 and 20mg Fluoxetine Capsules HPLC Determination
BACKGROUND
Therapeutically, Fluoxetine hydrochloride is a classified as a lective rotonin-reuptake inhibitor. Effectively ud for the treatment of various depressions. Fluoxetine hydrochloride has been shown to have comparable efficacy to tricyclic antidepressants but with fewer anticholinergic side effects. The patent expiry becomes effective in 2001 (US). INTRODUCTION
Fluoxetine capsules were prepared in two dosage strengths: 10mg and 20mg dosage strengths with the same capsule weight. The formulas are esntially similar and geometrically equivalent with the same ingredients and proportions. Minor changes in non-active proportions account for the change in active ingredient amounts from the 10 and 20 mg strength.
The following validation, for the method SI-IAG-206-02 , includes assay and determination of Meta-Fluoxetine by HPLC, is bad on the analytical method validation SI-IAG-209-06. Currently the method is the in-hou method performed for Stability Studies. The Validation was performed on the 20mg dosage samples, IAG-21-001 and IAG-21-002.
In the forced degradation studies, the two placebo samples were also ud. PRECISION
SYSTEM REPEATABILITY
Five replicate injections of the standard solution at the concentration of 0.4242mg/mL as described in method SI-IAG-206-02 were made and the relative standard deviation (RSD) of the peak areas was calculated.
SAMPLE PEAK AREA
#15390
the ting tings#25406
#35405
#45405
#55406
Average5402.7
SD 6.1
% RSD0.1
ED. N0: 04Effective Date:APPROVED::
HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.
ANALYTICAL METHOD VALIDATION
10 and 20mg Fluoxetine Capsules HPLC Determination
ED. N0: 04Effective Date:APPROVED::
PRECISION - Method Repeatability
as oneThe full HPLC method as described in SI-IAG-206-02 was carried-out on the finished product IAG-21-001 for the 20mg dosage form. The method repeated six times and the relative standard deviation (RSD) was calculated.
SAMPLE
Number
%ASSAY
of labeled amount
孔子英文I 96.9II 97.8III 98.2IV 97.4V 97.7VI 98.5(%) Average
97.7SD 0.6(%) RSD
0.6
PRECISION - Intermediate Precision
ome 103
The full method as described in SI-IAG-206-02 was carried-out on the finished product IAG-21-001 for the 20mg dosage form. The method was repeated six times by a cond analyst on a different day using a different HPLC instrument. The average assay and the relative standard deviation (RSD) were calculated.
fullversionSAMPLE
Number
% ASSAY
of labeled amount
I 98.3II 96.3III 94.6IV 96.3V 97.8VI 93.3Average (%)
wk是什么意思
96.1SD 2.0RSD (%)
2.1
The difference between the average results of method repeatability and the intermediate precision is 1.7%.
HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.
ANALYTICAL METHOD VALIDATION
10 and 20mg Fluoxetine Capsules HPLC Determination
LINEARITY
Standard solutions were prepared at 50% to 200% of the nominal concentration required by the assay procedure. Linear regression analysis demonstrated acceptability of the method for quantitati
ve analysis over the concentration range required. Y-Intercept was found to be insignificant.
RANGE
Different concentrations of the sample (IAG-21-001) for the 20mg dosage form were prepared, covering between 50% - 200% of the nominal weight of the sample.
Conc. (%)Conc. (mg/mL)Peak Area% Assay
of labeled amount
500.20116235096.7
700.27935334099.2
1000.39734463296.6
1500.64480757797.5
2000.79448939497.9
(%) Average97.6cup是什么意思
SD 1.0
(%) RSD 1.0
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