1. | METHOD DEVELOPMENT AND VALIDATION OF
SIMULTANEOUS ESTIMATION OF DROSPIRENONE AND
ESTETROL BY USING UV-SPECTROSCOPY |
| Garamsandh Gandhi V*, Manivannan R, Blessalya M, Boopathi S, Deepak Kumar A,
Harish K, Yaswanth PS |
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Ultraviolet and visible (UV-Vis) absorption spectroscopy is the measurement of the attenuation of a beamof light
after it passes through a sample or after reflection from a sample surface. Light energy is converted by detectors into
electrical impulses that are read out by readout devices. The transmitted radiation strikes the detector, determining the
amount of radiation absorbed by the sample. The absorption spectrophotometer's apparatus uses the following types of
detectors. Aim of the present study is to develop an accurate, precise, sensitive, selectivity, analyticaltechnique to determine
the Drospirenone and Estetrol in pharmaceutical dosage forms. Drospirenone is a progestin used in oral contraceptive pills for
the prevention of pregnancyand other conditions. Percentage of RSD for intra-day and inter-day precision studies for both
drugs were well within the acceptable range (< 2 %) indicating that the method have excellent repeatability and
reproducibility
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2. | NALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE
SIMULTANEOUS ESTIMATION OF DECITABINE AND CEDAZURIDINE IN
BULK AND PHARMACEUTICAL DOSAGE FORM BY RP-HPLC METHOD |
| Yamini S*1, Rajitha S |
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High performance liquid chromatography is at present one of the most sophisticated tool of the analysis. The estimation of
Decitabine and Cedazuridine was done by RP-HPLC. The Phosphate buffer was pH 4.5 and the mobile phase was optimized
with consists of Methanol: Phosphate buffer mixed in the ratio of PH 4.5(20:80 v/v). Kromosil C18 Column (250mm x
4.6mm)5µg or equivalent chemically bonded to porous silica particles was used as stationary phase. The detection was carried
out using UV detector at 254 nm. The solutions were chromatographed at a constant flow rate of 1 ml min-1. The linearity
range of Decitabine and Cedazuridine were found to be from 100-500 mg/ml of Decitabine and 1-5mg/ml of Cedazuridine.
Linear regression coefficient was not more than 0.999. The values of % RSD are less than 2% indicating accuracy and
precision of the method. Decitabine %RSD 0.2 and Cedazuridine %RSD 0.6. Intermediate precision for Decitabine %RSD 0.2
and Cedazuridine %RSD 0.1 The percentage recovery varies from 98-102% of Decitabine and Cedazuridine. LOD and LOQ
were found to be within limit. The results obtained on the validation parameters met ICH and USP requirements .it inferred the
method found to be simple, accurate, precise and linear. The method was found to be having suitable application in routine
laboratory analysis with high degree of accuracy and precision
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3. | NOVEL RP-HPLC TECHNIQUE FOR PRECISE ESTIMATION OF
SITAGLIPTIN AND DOSAGE FORM |
| Deepthi P, Mounika Grace B, Naveen B, Sowmya Sharon M, Visista N Vanitha T |
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Analytical method development and validation plays important role in the discovery, development and manufacture of
pharmaceuticals. HPLC mainly utilizes a column that holds packing material (stationary phase), a pump that moves the mobile
phase(s) through the column, and a detector that shows the retention times of the molecules. Sitagliptin is used for the
treatment of type 2 diabetes mellitus. It is prescribed as an adjunct to diet and exercise to improve glycemic control in adults.
Sitagliptin is anti-diabetic drug is more potent inhibitor of DPP-4. The present study was planned to estimate the drug present
in the tablets by developing and validating new RP-HPLC method. In chromatographic analysis of substances RP-HPLC is
normally advocated because of faster elution. The proposed RP-HPLC methods in construction with dissolution studies were
developed for the quantitative estimation of the Sitagliptin was found to be accurate, rapid, sensitive and economical
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4. | METHOD DEVELOPMENT FOR SIMULTANEOUS ESTIMATION OF
VILANTEROL TRIFENATATE AND FLUTICASONE FUROATE
USING RP-HPLC METHOD |
| Karpuram Prasanthi, Dinakar A, Sandhya K, Avinash Kumar G |
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A new RP-HPLC method was developed and validated for the simultaneous estimation of Vilanterol trifenatate and
Fluticasone furoate in bulk and pharmaceutical dosage forms. Chromatographic separation was achieved using a Waters BEH
C18 column (4.6×150mm, 5?m), with a mobile phase consisting of methanol:acetonitrile buffer (60:20:20 v/v) at a flow rate
of 1.0 ml/min, and detection at 280 nm. Retention times were 3.539 mins for Vilanterol trifenatate and 4.232 mins for
Fluticasone furoate. The method exhibited high system suitability parameters, including theoretical plates, tailing factors, and
resolution. The method was validated in accordance with ICH guidelines, demonstrating excellent linearity (r2=0.999 for both
compounds), accuracy, precision, and robustness. The linearity range was 50?g-250?g for Vilanterol trifenatate and 5?g-25?g
for Fluticasone furoate. Percentage recoveries were 99.56% and 99.48%, respectively, with %RSD for repeatability at 0.1 and
1.4. Intermediate precision %RSD for analysts 1 and 2 were within acceptable limits. LOD values were 0.39 ?g/ml and 0.7
?g/ml, and LOQ values were 1.18 ?g/ml and 2.12 ?g/ml for Vilanterol trifenatate and Fluticasone furoate, respectively. The
method was further validated through force degradation studies under various conditions, proving its stability-indicating
capability. This RP-HPLC method is suitable for routine quality control, stability studies, and simultaneous analysis of
Vilanterol trifenatate and Fluticasone furoate in pharmaceutical formulations
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5. | NOVEL RPHPLC METHOD DEVELOPMENT AND VALIDATION OF
SIMULTANEOUS ESTIMATION OF TOPIROXOSTAT AND
DOTINURAD |
| Lomada Nandini, Dinakar A2*, Sandhya K2, Avinash Kumar G |
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A novel reverse-phase high-performance liquid chromatography (RP-HPLC) method was designed and developed for the
simultaneous estimation of Topiroxostat and Dotinurad in synthetic mixtures. The method exhibited high accuracy, precision,
and robustness, making it ideal for routine analytical applications. Assay results demonstrated 99.93% for Topiroxostat and
99.95% for Dotinurad, indicating minimal error and reliable quantification of active pharmaceutical ingredients. Linearity
assessments revealed a correlation coefficient of 0.999 for both compounds, confirming excellent linearity and sensitivity
across a wide concentration range. The method showed remarkable precision with relative standard deviation (RSD) values of
0.6% for Topiroxostat and 0.8% for Dotinurad, well within the acceptance criteria of RSD not more than 2.0%. Intermediate
precision, with RSD values of 0.6% for both drugs, demonstrated the method's reliability across different days and analysts.
Accuracy was validated through recovery studies, yielding 99.60% for Topiroxostat and 100.15% for Dotinurad, within the
acceptable range of 97.0% to 103.0%, indicating reliable recovery of analytes. Limits of detection (LOD) were 3.07 ?g/mL for
Topiroxostat and 2.95 ?g/mL for Dotinurad, while limits of quantification (LOQ) were 10.09 ?g/mL and 9.93 ?g/mL,
respectively, showcasing the method's capability for trace analysis. Robustness testing confirmed consistent performance
under varied mobile phase composition and flow rate conditions. The method's robustness and system suitability, coupled with
high precision and accuracy, underscore its potential for routine quality control, dissolution studies, and bioequivalence
assessments of formulations containing Topiroxostat and Dotinurad
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