Research Article - (2011) Volume 2, Issue 9

Development and Validation of a Stability Indicating UPLC Method for Determination of Moxifloxacin Hydrochloride in Pharmaceutical Formulations

G. Naveen Kumar Reddy1*, V.V.S.Rajendra Prasad2, Nigam Jyoti Maiti3, Diptimayee Nayak3 and Prashant Kumar Maharana4
1Singhania University, Pacheri Bari, Jhunjhunu, Rajasthan, India
2Sitha Institute of Pharmaceutical Sciences, jntu, Hyderabad, India
3Department of Pharmacy, IMT College of Pharmacy, Puri, Odisha, India
4Mannequin Pharmaceutical, Bhubaneshwar, Odisha, India
*Corresponding Author: G. Naveen Kumar Reddy, Singhania University, Pacheri Bari, Jhunjhunu, Rajasthan, India, Tel: +91996340443 Email:

Abstract

Simple, rapid, sensitive, accurate, robust & rugged stability indicating analytical method for determination of Moxifloxacin HCl in pharmaceutical formulations is developed and validated by using UPLC & applied the developed and validated method for determining the assay of Moxifloxacin HCl in tablets (Avelox®), as there is no official monograph & no analytical method by UPLC. Chromatography was performed with mobile phase containing potassium dihydrogen ortho phosphate (adjusted to pH 1.8 with orthophosphoric acid), Methanol & acetonitrile in the ratio of 60:20:20, with a flow rate of 0.3mL/min, C-18 column & UV detection at 296nm.The method was validated for linearity, accuracy, ruggedness, robustness, precision & bench top stability of sample & standard solution. Moxifloxacin tablets were subjected to different stress conditions like acid, alkali, peroxide, thermal, water & UV studies and checked for its specificity, degradation & stability. The developed method was very rapid with a run time of 3 min, accurate, robust, rugged and stable.

Keywords: Moxifloxacin; Assay method; UPLC; Stability indicating method

Introduction

Ultra performance liquid chromatography (UPLC) takes advantage of technological strides made in particle chemistry performance, system optimization, detector design, and data processing and control. Using sub-2 mm particles and mobile phases at high linear velocities, and instrumentation that operates at higher pressures than those used in HPLC, dramatic increases in resolution, sensitivity, and speed of analysis can be obtained. This new category of analytical separation science retains the practicality and principles of HPLC while creating a step function improvement in chromatographic performance [1].

According to an FDA guidance document, a stability-indicating method is “a validated quantitative analytical procedure that can detect the changes with time in the pertinent properties of the drug substance and drug product. A stability-indicating method accurately measures the active ingredients, without interference from degradation products, process impurities, excipients, or other potential impurities” [2].

Moxifloxacin is slightly yellow crystalline mono-hydrochloride salt [3]. Moxifloxacin Hydrochloride is designated chemically as ((1’S,6’S)-1-Cyclopropyl-7-(2,8-diazabicyclo[4.3.0]non-8-yl)-6- fluoro-8-methoxy-4-oxo-1,4-dihydroquinoline-3-carboxylic acid hydrochloride (Figure 1) [4]. Moxifloxacin can be used to treat respiratory infections, including acute sinusitis, acute exacerbations of chronic bronchitis, and community-acquired pneumonia, as well as skin and skin structure infections. Moxifloxacin is also used for the treatment of complicated intra-abdominal infections [5]. Moxifloxacin inhibits bacterial topoisomerase II (DNA gyrase) and topoisomerase IV. Topoisomerases are essential enzymes which play a crucial role in the replication and repair of bacterial DNA. This mechanism is lethal to susceptible bacteria. Moxifloxacin is often referred to as a chemotherapeutic drug because its mode of action has so far not been noted in any naturally occurring or semi-synthetic antibiotic.

pharmaceutica-analytica-acta-Moxifloxacin-Hydrochloride

Figure 1: Moxifloxacin Hydrochloride.

A few methods for the determination of Moxifloxacin Hydrochloride in pharmaceutical formulations by HPLC [6], HPTLC [3] and UV [7] appear in literature. So far no systematic UPLC method has been reported for determination of Moxifloxacin Hydrochloride in pharmaceutical formulations. This paper reports a rapid and sensitive UPLC method with UV detection, useful for routine quality control of Moxifloxacin Hydrochloride in pharmaceutical formulations. The method was validated by parameters such as linearity, accuracy, precision, robustness, ruggedness, sample and standard solution stability and forced degradation studies.

Experimental

Reagents

HPLC grade Acetonitrile (HPLC Grade, Merck), Potassium dihydrogen orthophosphate (AR, Rankem), Hydrochloric Acid (AR, Rankem) Sodium hydroxide (AR, Rankem), Hydrogen peroxide (AR, Rankem), Ortho phosphoric acid (AR,Rankem),Water (Milli Q water), Acetonitrile (HPLC Grade, Merck). Moxifloxacin pure drug substance was kindly supplied by MSN Laboratories Limited, India. Ingredients used for placebo were microcrystalline cellulose, croscarmellose sodium, PVPK-30, Ethanol, Magnesium stearate.

Instrumentation

A liquid chromatography (Waters Acquity) system equipped with an injection valve (Rheodyne) & PDA detector. The UPLC system was well equipped with Empower 2 software for data processing. Other instruments like Sartorius Analytical Balance, Metrohm pH Meter and Biotechnics sonicator were used in sample and standard preparations and for forced degradation studies.

Methodology

Chromatographic conditions

The analytical column used was Waters HSS, C-18, 100X2.1; 1.8μm .The mobile phase was potassium dihydrogen ortho phosphate, adjusted to pH 1.8 with ortho phosphoric acid, methanol & acetonitrile in the ratio of 60:20:20. It has a flow rate of 0.3mL/min, injection volume of 1μL with ambient column oven temperature and sample tray temperature with isocratic elution & UV detection at 296nm & a run time of 3 min.

Standard, sample, mobile phase and diluent preparation

Diluent: Mobile phase is used as diluent:

Preparation of mobile phase: Dissolved 3.4g of potassium dihydrogen ortho phosphate in one litre water and adjusted the pH to 1.8 with ortho phosphoric acid.Filtered through 0.22μ membrane filter. Mixed the buffer,acetonitrile and methanol in the ratio of 60:20:20 and sonicated to degas.

Preparation of standard solution: Accurately weighed and transferred 44mg of Moxifloxacin HCl in to a 100mL volumetric flask and added 70mL of diluent.Sonicated for 5 min and made up to the mark with diluent.Transferred 5mL of above solution to 20mL volumetric flask and made up to volume with diluent. Filtered with 0.45μm PFTE filter.

Preparation of Test solution: Weighed 20 tablets(Avelox-400mg) manufactured by Bayer Health Care AG, Germany and determined the average weight.Weighed 2 tablets and transferred in to a 200mL volumetric flask and added 150mL of diluent.Sonicated in cold water for 20minutes with intermittent shaking.Allowed it to cool to room temperature and diluted to volume with diluent. Filtered atleast 12mL of the above solution with 0.45μm PTFE filter and transfered 5mL of filtered solution to 200mL volumetric flask and made up to volume with diluent.

Method development

By selecting the HPLC method conditions from literature and by using the UPLC method convertor calculated the chromatographic conditions.

Wavelength was selected at 296nm based on the literature [6] and by scanning with PDA detector.

pH of the buffer was selected based on its pKa value.

Taken 0.05M Potassium di hydrogen phosphate and adjusted the pH to1.8±0.05 with OPA. By using buffer and ACN: MeOH (600:400) and by using the gradient programmes mentioned as in (Table 1) with HSS C-18,100X2.1,1.8μm column, flow rate of 0.3mL/min, injection volume(5μl),column oven temperature at 25°C injected the Moxifloxacin HCl standard.

Trial-1 Trial-2 Trial-3
Time Buffer
 % A
ACN:MeOH
      % B
Time Buffer
 % A
ACN:MeOH
       % B
Time Buffer
 % A
ACN:MeOH
      % B
0.00 100 0 0.00 85 15 0.00 70 30
10.00 95 5 10.00 85 15 3.50 70 30
15.00 85 15 15.00 57 46 4.50 30 70
30.00 70 30 30.00 56 44 5.50 70 30
40.00 40 60 40.00 30 70 7.00 70 30
345.00 100 0 45.00 85 15      
50.00 100 0 50.00 85 15      

Table 1

In Trial -1 a split peak was observed at a retention time 34min, which might be because of more buffer. So changed the gradient programme with less buffer and more organic solvents as in Trial -2, in this case the peak was little broad and the retention time decreased to 7min.Then decreased the buffer as mentioned in Trial-3 and with that gradient programme and with an injection volume of 1μL injected Moxifloxacin HCl standard. In this it eluted at 3.2RT and the peak shape was good.

By considering all the aspects went for an isocratic elution with Buffer : (ACN: MeOH) 600:400 and with the above mentioned chromatographic conditions injected standard and test solutions. Peak shape, theoretical plates, RSD and tailing all were fine and within the limits.

Results and Discussion

Specificity

Specificity is the ability to assess unequivocally the analyte in the presence of components which may be expected to be present. Typically these might include impurities, degradants, matrix, etc. [8]. Specificity was demonstrated by injecting a blank, placebo and standard solution. No interference was seen at the retention time of analyte. The specificity was also demonstrated by induced degradation of Moxifloxacin formulation and placebo samples to acid degradation, alkali degradation, peroxide degradation, thermal degradation, water degradation, U.V. degradation. Purity angle is less than purity threshold for all the stress conditions. The results are tabulated in (Table 2), (Figures 2-15) represents different stress conditions.

MOXIFLOXACIN FORCED DEGRADATION
Stress Condition Reagent Used Conc. Purity Angle Purity Threshold
Acid Stress HCl 0.1N 0.120 0.271
Alkali Stress NaOH 0.1N 0.124 0.274
Peroxide Stress H2O2 3% 0.138 0.297
Water Stress Water   0.140 0.277
Heat Stress Heater 60°C 0.118 0.272
U.V. Stress Photolytic
chamber
1 Week 0.170 0.278
Acceptance Criteria Peak Purity shall pass

Table 2

pharmaceutica-analytica-acta-Blank-Diluent

Figure 2: Blank-Diluent.

pharmaceutica-analytica-acta-Standard

Figure 3: Standard.

pharmaceutica-analytica-acta-Acid-Stressed-Placebo

Figure 4: Acid Stressed Placebo Solution.

pharmaceutica-analytica-acta-Alkali-Stressed-Placebo

Figure 5: Alkali Stressed Placebo.

pharmaceutica-analytica-acta-Peroxide-Stressed-Placebo

Figure 6: Peroxide Stressed Placebo.

pharmaceutica-analytica-acta-Water-Stressed-Placebo

Figure 7: Water Stressed Placebo.

pharmaceutica-analytica-acta-Heat-Stressed-Placebo

Figure 8: Heat Stressed Placebo.

pharmaceutica-analytica-acta-UV-Stressed-Placebo

Figure 9: UV Stressed Placebo.

pharmaceutica-analytica-acta-Acid-Stressed-Sample

Figure 10: Acid Stressed Sample.

pharmaceutica-analytica-acta-Alkali-Stressed-Sample

Figure 11: Alkali Stressed Sample.

pharmaceutica-analytica-acta-Peroxide-Stressed-Sample

Figure 12: Peroxide Stressed Sample.

pharmaceutica-analytica-acta-Water-Stressed-Sample

Figure 13: Water Stressed Sample.

pharmaceutica-analytica-acta-Heat-Stressed-Sample

Figure 14: Heat Stressed Sample.

pharmaceutica-analytica-acta-UV-Stressed-Sample

Figure 15: UV Stressed Sample.

System suitability Testing

System suitability testing is used to verify that the reproducibility of the system is adequate for the analysis to be performed. System suitability is done by preparing and injecting the standard solution 5 times and calculating its RSD. Other parameters like tailing and theoretical plates should also be taken in to consideration. Results are tabulated in (Table 3).

Moxifloxacin System Suitability
Injection No.: 1 2 3 4 5 Mean STDEV RSD Limits
Standard Area: 2305687 2302824 2311478 2300543 2283295 2300765 10589 0.5 RSD NMT 2.0%
Theoretical Plates 7818 7835 7825 7826 7829 7827 6.19 0.1 NLT 2000
USP tailing 1.54 1.54 1.54 1.54 1.53 1.54 0.00 0.3 NMT 2.0
RT 1.259 1.260 1.263 1.265 1.267 1.263 0.00 0.3  

Table 3

Linearity

The linearity of an analytical procedure is its ability (within a given range) to obtain test results which are directly proportional to the concentration (amount) of analyte in the sample [8]. The linearity of the test method was performed by plotting a graph between concentration of the test solution on X-axis and response of the corresponding solutions on Y-axis from 40% to 160% of test concentration and calculated the correlation coefficient, it was found to be 0.999.The results are tabulated in (Table 4 and 5) and the graphs are represented as Figure 16.

Moxifloxacin
Weighed
Equivalent
to mg
MOXIFLOXACIN-LINEARITY
Diluted to(mL) mL mL Conc. (µg/mL)
43.64 40.02 100 2 20 40.02
43.64 40.02 100 4 20 80.04
43.64 40.02 100 5 20 100.04
43.64 40.02 100 6 20 120.05
43.64 40.02 100 8 20 160.07

Table 4

MOXIFLOXACIN-LINEARITY
Run % Conc. Conc. Of
Moxifloxacin
(µg/mL)
Area of
Moxifloxacin
Slope Y-intercept R2
1 40% 40.02 937722 23058.3 27292.95 0.999
80% 80.04 1908256
100% 100.04 2295800
120% 120.05 2819056
160% 160.07 3709937
2 40% 40.02 942173 23183.8 25535.15 0.999
80% 80.04 1908189
100% 100.04 2301865
120% 120.05 2852614
160% 160.07 3719921
3 40% 40.02 943469 23069.1 31258.15 0.999
80% 80.04 1902911
100% 100.04 2306901
120% 120.05 2831549
160% 160.07 3711182
Average 23103.74846 28028.75 0.999
Standard Deviation 69.55 2931.59 0.00
Acceptance criteria: Coefficient of correlation shall be NLT 0.999

Table 5

pharmaceutica-analytica-acta-Linearity

Figure 16: Linearity.

Limit of detection (LOD) and limit of quantification (LOQ)

The detection limit of an individual analytical procedure is the lowest amount of analyte in a sample which can be detected but not necessarily quantitated as an exact value. The quantitation limit of an individual analytical procedure is the lowest amount of analyte in a sample which can be quantitatively determined with suitable precision and accuracy [8]. Calculated the LOD & LOQ, with the calculations obtained from evaluation of the calibration curve of the linearity. LOD and LOQ values are less than the minimum linearity concentration.

The calculations and results are tabulated in (Table 6).

Moxifloxacin- Limit of detection (LOD) & Limit of Quantification (LOQ)
S.No. Injection No. Slope Y-Intercept R2
1 Inj-1 23059.4 27156.504 0.999
2 Inj-2 23184.9 25399.4381 0.999
3 Inj-3 23070.2 31121.98583 0.998
Average 23104.8333 27892.6426 0.9987
STDEV 69.550 2931.435 0.001
LOD=3.3 x σ/S
LOD 0.4 ppm    
LOQ=10 x σ/S
σ = Standard deviation of y-intercepts of regression line
S= slope of the linearity curve
LOQ 1.3 ppm    
Acceptance Criteria: LOD & LOQ values shall be less than the minimum linearity concentration

Table 6

Bench top stability of standard & test preparation

Performed the assay of Moxifloxacin as per the test method in duplicate and kept the standard and test solutions on the bench top for 48 Hrs. Injected at initial, 24 Hrs. and 48 Hrs. Calculated the difference between initial and bench top stability samples for % assay of Moxifloxacin for test solutions and similarity factor for standard solutions were found to be within limits. The results are tabulated in (Table 7).

Moxifloxacin Bench Top Stability of Standard Solution
Time(Hrs) Day Std. Wt. Response Fresh Std Wt. Response of
 fresh std.
Similarity
 Factor
Initial Initial 44.02 2300765      
24 Hrs Day-1 44.02 2311082 44.13 2316978 1
48 Hrs Day-2 44.02 229288 43.89 2268919 0.99
Acceptance Limits: Similarity Factor should be NMT 2.0
             
Moxifloxacin Bench Top Stability of Test Solution-1
Time(Hrs) Day Weight(mg) Response
 of sample
% Assay Difference from Initial Difference in Assay results of Initial,24 & 48 Hrs shall be NMT 2.0
Initial Initial 1353.34 2337254 101.29 NA
24 Hrs Day-1 1353.34 2331881 100.6 0.7
48 Hrs Day-2 1353.34 2305445 101.01 0.3
             
Moxifloxacin Bench Top Stability of Test Solution-2
Time(Hrs) Day Weight(mg) Response
 of sample
% Assay Difference from Initial Difference in Assay results of Initial,24 & 48 Hrs shall be NMT 2.0
Initial Initial 1351.89 2321427 100.6 NA
24 Hrs Day-1 1351.89 2320794 100.12 0.5
48 Hrs Day-2 1351.89 2327728 101.99 1.4

Table 7

Accuracy

The accuracy of an analytical procedure expresses the closeness of agreement between the value which is accepted either as a conventional true value or an accepted reference value and the value found [8]. Performed the accuracy of test method using Moxifloxacin placebo at 50%, 70%, 100%, 125%, 150% spike levels. The % assay at each spike level was found to be between 98.0-102.0% of the labeled amount. The results are tabulated in (Table 8 and 9).

Standard
Preparation
44.13 mg 5 Potency 98.8    
100   20        
            Molecular factor
 of Moxifloxacin
 
Sample
 Preparation
Wt. of sample taken in mg 5 Label Claim 400 0.917
200   200        
               
Standard Area 2316978   Average Wt. in mg   675.01  

Table 8

MOXIFLOXACIN-ACCURACY
Spike
level
Wt.of sample
taken in mg
Sample
 area
mg/mL
added
mg/mL
found
% Recovery % Recovery Average
50%_01 674.46 1159290 0.04996 0.05454 100.1 100.1 100.1
50%_02 672.90 1155954 0.04984 0.05438 100.1 100.0
50%_03 673.11 1158198 0.04986 0.05449 100.2 100.2
70%_01 1018.65 1753515 0.07545 0.08249 100.3 100.3 100.0
70%_02 1018.42 1746671 0.07544 0.08217 99.9 99.9
70%_03 1016.46 1744562 0.07529 0.08207 100.0 100.0
100%_01 1349.09 2292178 0.09993 0.10783 98.9 99.0 98.6
100%_02 1348.20 2281190 0.09987 0.10732 98.5 98.5
100%_03 1347.63 2272375 0.09982 0.10690 98.2 98.2
125%_01 1686.17 2867979 0.1249 0.13492 99.1 99.1 98.9
125%_02 1685.31 2856118 0.12484 0.13436 98.7 98.7
125%_03 1685.91 2866778 0.12488 0.13487 99.0 99.0
150%_01 2015.68 3400552 0.14931 0.15998 98.3 98.3 98.2
150%_02 2023.69 3406155 0.1499 0.16024 98.0 98.0
150%_03 2021.14 3411601 0.14971 0.16050 98.3 98.3

/td>

Acceptance criteria:% Average recovery shall be  between 98.0% -102.0%

Table 9

Precision

The precision of an analytical procedure expresses the closeness of agreement (degree of scatter) between a series of measurements obtained from multiple sampling of the same homogeneous sample under the prescribed conditions. Precision may be considered at three levels: repeatability, intermediate precision and reproducibility [8].

Method precision

Determined the precision of the test method by preparing & injecting 6 test solutions of Moxifloxacin formulations in to the chromatograph and recorded the results. The average % assay was found to be 100.4 with % RSD of 0.62. The results are tabulated in (Table 10).

Moxifloxacin Analytical Method Validation-Assay
Method Parameter Method Precision
Std. wt. &
Dilution
44.02 5 Tablet Wt. Spl. wt. &
Dilution
Wt. of sample
 taken
5 Label claim
(mg)
400
100 20 675.01 200 200 Potency (%) 98.8
Molecular factor for Moxifloxacin 0.917        
Std. No. Standards USP
 Tailing
Weight of
sample taken
Area of
sample
Assay % Average
      (%)
STDEV % RSD
1 2310915 1.54 1353.34 2337254 101.04 100.4 0.61837 0.62
2 2290693 1.54 1351.89 2321427 100.46
3 2300684 1.54 1358.15 2317128 99.81
4 2300777 1.54 1353.97 2341249 101.16
5 2300755 1.54 1355.02 2324067 100.34
      1356.39 2310208 99.64
Average 2300765 1.54 1354.79 2325222 100.41
STDEV 7149.73 0.00 Limits % RSD of 6 replicate injections is not more than 2
%RSD 0.31 0.0

Table 10

Intermediate precision

Performed the assay of Moxifloxacin by following the same procedure as that of Method precision but on a different day and by a different analyst. The average % assay was found to be 99.4% with % RSD of 0.39.Overall RSD when compared with Method precision is 0.73. The results are tabulated in (Table 11 and 12).

Moxifloxacin Analytical Method Validation-Assay
Method Parameter Intermediate Precision
Std. wt. &
Dilution
44.13 5 Tablet Wt. Sample wt. &
Dilution
Wt. of sample
 taken
5 Label claim
(mg)
400
100 20 675.01 200 200 Potency (%) 98.8
Molecular factor for Moxifloxacin 0.917        
Std. No. Standards USP
 Tailing
Wt. of
sample taken
Area of
sample
Assay % Average              
   (%)
STDEV % RSD
1 2315498 1.52 1351.91 2303175 99.22 99.4 0.388 0.39
2 2302693 1.52 1360.40 2318575 99.26
3 2314434 1.52 1355.75 2314650 99.43
4 2321577 1.52 1353.39 2305262 99.20
5 2330688 1.52 1352.51 2325271 100.13
6     1356.55 2306776 99.03
Average 2316978 2 1355 2312285 99.38
STDEV 10269.35 0.00 Limits % RSD of 6 replicate injections is not more than 2
%RSD 0.4 0.0

Table 11

Moxifloxacin Analytical Method Validation-Assay
Method Parameter Method & Intermediate Precision combined
Method Precision   Intermediate Precision        
S.No. % Drug
 content
S.No. % Drug
 content
Difference Average of both
Method &
Intermediate
 precision
STDEV of both
Method &
Intermediate
 precision
%RSD of both
Method &
Intermediate
 precision
1 101.04 1 99.2 1.8 99.9 0.730 0.73
2 100.46 2 99.3 1.2
3 99.81 3 99.4 0.4
4 101.16 4 99.2 2.0
5 100.34 5 100.1 0.2
6 99.64 6 99.0 0.6
Limits: Overall RSD when compared with Method precision should be not more than 2%.

Table 12

Robustness

The robustness of an analytical procedure is a measure of its capacity to remain unaffected by small, but deliberate variations in method parameters and provides an indication of its reliability during normal usage [8]. Robustness was performed by injecting the Moxifloxacin standard solution in to the UPLC by altering the Flow rate, Column oven temperature and also by changing the pH of the buffer & composition of the organic solvent from the normal chromatographic conditions. The results are tabulated in (Table 13).

Moxifloxacin Analytical Method Validation-Assay
Method Parameter Robustness
Change in Flow Rate(0.25mL/min) Change in Flow Rate(0.35mL/min)
Std. No. Standards USP
 Tailing
Std. No. Standards USP
 Tailing
1 2743760 1.55 1 1973875 1.49
2 2774673 1.55 2 1943344 1.49
3 2740829 1.55 3 1960245 1.49
4 2732432 1.55 4 1952056 1.49
5 2734277 1.55 5 1958542 1.49
Average 2745194 1.55 Average 1957612 1.49
STDEV 17118.49 0.00 STDEV 11255.31 0.00
%RSD 0.62 0.0 %RSD 0.57 0.0
 
Change in pH of Mobile Phase(1.6) Change in pH of Mobile Phase(2.0)
Std. No. Standards USP
 Tailing
Std. No. Standards USP
 Tailing
1 2271424 1.49 1 2263481 1.53
2 2252217 1.49 2 2258739 1.53
3 2249439 1.49 3 2276006 1.53
4 2244184 1.49 4 2272593 1.53
5 2241573 1.48 5 2276184 1.53
Average 2251767 1.49 Average 2269401 1.53
STDEV 11762.64 0.00 STDEV 7882.71 0.00
%RSD 0.52 0.3 %RSD 0.35 0.0
           
Change in Org Phase Composition (90%) Change in Org Phase Composition (110%)
Std. No. Standards USP
 Tailing
Std. No. Standards USP
 Tailing
1 2311223 1.43 1 2265737 1.53
2 2313683 1.43 2 2269570 1.53
3 2305552 1.43 3 2290266 1.53
4 2315524 1.43 4 2291368 1.53
5 2306395 1.43 5 2290691 1.53
Average 2310475 1.43 Average 2281526 1.53
STDEV 4393.90 0.00 STDEV 12742.53 0.00
%RSD 0.19 0.0 %RSD 0.56 0.00

Table 13

Calculation:

Equation

Where

At=Area of test solution; P=Potency of Moxifloxacin HCl Working Std.on as is basis

As=Area of standard solution; Avg. Wt. =Avg. Wt. of 20 tablets

Ws=Weight of standard taken; LC=Label claim of the tablet as Moxifloxacin

Wt=Weight of two tablets; MF=Molecular Factor for Moxifloxacin (0.917)

Conclusion

The reported UPLC method was proved to be simple, rapid with a runtime of 3 min & reproducible. The validation data indicates good specificity, precision, accuracy & reliability of the method. The developed method has many advantages like isocratic mode of elution, easy sample preparation, short run time and can be used for routine quality control analysis of Moxifloxacin formulations.

References

Citation: Naveen Kumar Reddy G, Rajendra Prasad VVS, Maiti NJ, Nayak D, Prashant Kumar M (2011) Development and Validation of a Stability Indicating UPLC Method for Determination of Moxifloxacin Hydrochloride in Pharmaceutical Formulations. Pharm Anal Acta 2:142.

Copyright: © 2011 Naveen Kumar Reddy G, et al. This is an open-access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.