DEVELOPMENT AND VALIDATION OF RP-UPLC METHOD USING EXPERIMENTAL DESIGN APPROACH FOR SIMULTANEOUS ESTIMATION OF CANDESARTAN CILEXETIL AND CHLORTHALIDONE

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (11) ◽  
pp. 36-46
Author(s):  
M Singhal ◽  
◽  
S Amin ◽  
A Kukrety ◽  
A Chauhan ◽  
...  
Keyword(s):  
Candesartan Cilexetil ◽  
Ultra Performance Liquid Chromatography ◽  
Reversed Phase ◽  
Detector Response ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Ich Guidelines ◽  
Normal Probability ◽  
Development And Validation ◽  
Liquid Chromatographic

Candesartan Cilexetil is an antihypertensive agent currently available in combination with Hydrochlorothiazide. However, it has been proven by research that half dose of Chlorthalidone is equipotent to the dose of Hydrochlorothiazide in similar combination with Candesartan Cilexetil. At present there is no Liquid Chromatographic (LC) method available for the simultaneous estimation of Candesartan Cilexetil and Chlorthalidone in pharmaceutical dosage form. A simple, rapid, reliable and robust reversed phase ultra-performance liquid Chromatography (RP-UPLC) method was developed as per International Conference on Harmonization (ICH) guidelines. The best separation was achieved in less than 5 minutes on a 50 × 2.1 mm, 2.2 µm particle size Dionex C18 column with the gradient mobile phase 5 mM, 6.2 ± 0.5 pH ammonium acetate buffer - acetonitrile at a flow rate of 0.5 mL/min at 215nm. The detector response was linear in the range of 10-200 ppm of these drugs. LOD obtained was 3.04 ppm for Candesartan Cilexetil, 2.82 ppm for Chlorthalidone. Further evaluation of robustness of this method was carried out using Plackett-Burman verification with four factors two levels (high & low) within analytical QbD-principles using statistical software. The outcome of normal probability and overall desirability plots were found acceptable.

Development and Validation of Spectrophotometric and Liquid Chromatographic Methods for Estimation of Tigecycline in Injections

2020 ◽  
Vol 13 (5) ◽  
pp. 5148-5154
Author(s):  
Sagar Suman Panda ◽  
Ravi Kumar B.V.V.
Keyword(s):  
Area Under The Curve ◽  
Reversed Phase ◽  
Equal Concentration ◽  
Pharmaceutical Dosage Form ◽  
Liquid Chromatographic Method ◽  
Array Detection ◽  
The Difference ◽  
The One ◽  
Development And Validation ◽  
Liquid Chromatographic

Three new analytical methods were optimized and validated for the estimation of tigecycline (TGN) in its injection formulation. A difference UV spectroscopic, an area under the curve (AUC), and an ultrafast liquid chromatographic (UFLC) method were optimized for this purpose. The difference spectrophotometric method relied on the measurement of amplitude when equal concentration solutions of TGN in HCl are scanned against TGN in NaOH as reference. The measurements were done at 340 nm (maxima) and 410nm (minima). Further, the AUC under both the maxima and minima were measured at 335-345nm and 405-415nm, respectively. The liquid chromatographic method utilized a reversed-phase column (150mm×4.6mm, 5µm) with a mobile phase of methanol: 0.01M KH2PO4 buffer pH 3.5 (using orthophosphoric acid) in the ratio 80:20 %, v/v. The flow rate was 1.0ml/min, and diode array detection was done at 349nm. TGN eluted at 1.656min. All the methods were validated for linearity, precision, accuracy, stability, and robustness. The developed methods produced validation results within the satisfactory limits of ICH guidance. Further, these methods were applied to estimate the amount of TGN present in commercial lyophilized injection formulations, and the results were compared using the One-Way ANOVA test. Overall, the methods are rapid, simple, and reliable for routine quality control of TGN in the bulk and pharmaceutical dosage form. 

Development and Validation of the Analytical method for the estimation of a combination of 5-fluorouracil and Imiquimod by RP-HPLC

2021 ◽  
pp. 3313-3318
Author(s):  
Bhupender Tomar ◽  
Ankita Sharma ◽  
Inder Kumar ◽  
Sandeep Jain ◽  
Pallavi Ahirrao
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Ingredients ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, precise, and accurate reverse phase high performance liquid chromatographic method (RP-HPLC) was developed and validated for the estimation of the combination of 5- Fluorouracil (5-FU) and Imiquimod in active pharmaceutical ingredients (APIs). The method was carried out on Phenomenex C18 (250 × 4.6mm I.D., 5𝜇m) using isocratic elution mode. The mobile phase was used as Acetonitrile: 10mM potassium dihydrogen orthophosphate: triethylamine (40:59.9:0.1, v/v, pH 4.5 with orthophosphoric acid) and Water: ACN (50:50 v/v) was used as a diluent. The concentration of solvents was 1-20µg/ml and the volume of injection was 20µl with the flow rate of 1.2ml/min. The retention times for 5-FU and Imiquimod were found to be 1.9±0.5 and 6.6±0.5 min respectively. The absorption maxima of 5FU and Imiquimod were found 267nm and 227nm respectively. The method was validated as per ICH guidelines. All the data were found within the specified limits. The limit of detection (LOD) and limit of quantification (LOQ) of 5- Fluorouracil were found to be 0.015μg/mL and 0.048 μg/mL, respectively, and Imiquimod was found to be 0.078μg/mL and 0.237μg/mL, respectively. The method developed in the present study was found to be sensitive, specific, and precise and can be applied for the simultaneous estimation of 5-FU and Imiquimod.

DEVELOPMENT, VALIDATION OF RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF TENOFOVIR DISPROXIL FUMARATE, EMTRICITABINE AND RILPIVIRINE HYDROCHLORIDE IN BULK, FORMULATION AND USED IN NANOSUSPENSION

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (09) ◽  
pp. 43-54
Author(s):  
K Vijaya Sri ◽  
M. Madhuri ◽  
V. Anusha ◽  
V.R.K. Siresha ◽  
Keyword(s):  
Research Work ◽  
Multicomponent System ◽  
Hplc Method ◽  
Combination Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Line Of Therapy ◽  
Development And Validation

The present research work illustrates the development and validation of RP HPLC method for simultaneous estimation of tenofovir disproxil fumarate, emtricitabine and rilpivirine hydrochloride in bulk and formulated in a pharmaceutical dosage form as a nanosupension. Antiretroviral drug treatment is the primary line of therapy for treating HIV. The multicomponent system formulated as a nanosuspension evidenced increased hydrophilicity, potency and decreased side effects. The separation was carried out by using efficient BDS hypersil C18 HPLC column with empower software. Combination method of Precipitation—ultrasonic homogenization was used for the preparation of the nanosuspension. The mobile phase used was methanol, water, acetonitrile (80:13.4:6.6) v/v and flow rate 1mL /min. The developed method was thus validated as per ICH guidelines for various parameters whose results advocated the reliability of the method. The results for parameters viz. retention times of tenofovir disproxil fumarate, emtricitabine and rilpivirine were 3.09 min, 2.78 min and 3.68 min, linearity range was between 7.5-90, 5-60, 0.625-7.5µg/mL, respectively. Thus the new RP-HPLC method is optimum, reliable and can be used for the simultaneous estimation of tenofovir disproxil fumarate, emtricitabine and rilpivirine hydrochloride.

scholarly journals Simultaneous Estimation of Glimepiride, Rosiglitazone and Pioglitazone Hydrochloride in the Pharmaceutical Dosage Form

2010 ◽  
Vol 7 (4) ◽  
pp. 1326-1333 ◽  
Author(s):  
Freddy H. Havaldar ◽  
Dharmendra L. Vairal
Keyword(s):  
Dosage Form ◽  
Pharmaceutical Preparation ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Constant Flow Rate ◽  
Phase Liquid ◽  
Liquid Chromatographic

A simple, specific, accurate and economical gradient reversed phase liquid chromatographic (RP-HPLC) method was developed and subsequently validated for the determination of glimipiride, rosiglitazone and pioglitazone hydrochloride. Separation was achieved with a nucleodur C–18 column having 250×4.6 mm i.d. with 5 µm particle size and water HPLC grade adjusted to pH 3.0 using diluted orthophosphoric acid and acetonitrile (80:20 v∕v) with gradient program as eluent at a constant flow rate of 0.8 ml per min. UV detection was performed at 215 nm. The retention time of glimipiride, rosiglitazone and pioglitazone hydrochloride were about 17.9 min, 6.31 min and 8.24 min respectively. This method is simple, rapid and selective and can be used for routine analysis of antidiabetic drugs in pharmaceutical preparation. The proposed method was validated and successfully used for estimation of glimipiride, rosiglitazone and pioglitazone hydrochloride in the pharmaceutical dosage form.

Development and Validation of a Reversed-Phase Ultra-Performance Liquid Chromatographic Method for the Simultaneous Determination of Six Drugs Used for Combined Hypertension Therapy

2013 ◽  
Vol 96 (2) ◽  
pp. 295-300 ◽  
Author(s):  
Harshad O Kaila ◽  
Mrunal A Ambasana ◽  
Anamik K Shah
Keyword(s):  
Mobile Phase ◽  
Reversed Phase ◽  
Assay Method ◽  
Detector Response ◽  
Simultaneous Estimation ◽  
Good Resolution ◽  
Amlodipine Besylate ◽  
Hypertension Therapy ◽  
Liquid Chromatographic ◽  
Lercanidipine Hydrochloride

Abstract A simple, rapid, and reliable ultra-performance LC assay method has been developed for the simultaneous estimation of orally administered hypertension drugs (atenolol, hydrochlorothiazide, amlodipine besylate, indapamide, nifedipine, and lercanidipine hydrochloride), any of which may be administered with atenolol in combined hypertension therapy. Chromatography was carried out at 25°C on a 2.1 × 50 mm id, 1.7 μm particle size Acquity BEH C18 column with the isocratic mobile phase 0.01 M, 4.0 pH aqueous phosphate buffer–acetonitrile (50 + 50, v/v) at a flow rate of 0.35 mL/min. All drugs were separated in less than 4 min with good resolution and minimal tailing, without interference by excipients. The method was validated according to International Conference on Harmonization guidelines, and the acceptance criteria for accuracy, precision, linearity, specificity, and system suitability were met in all cases. The column effluent was monitored at 230 nm. The detector response was linear in the range of 1–20 μg/mL of these drugs. LOD obtained was 0.04 μg/mL for atenolol, 0.02 μg/mL for hydrochlorothiazide, 0.03 μg/mL for amlodipine besylate, 0.03 μg/mL for indapamide, 0.02 μg/mL for nifedipine, and 0.01 μg/mL for lercanidipine hydrochloride. The suggested method has the advantage that all the drugs can be quantified alone or in combination with atenolol using a single mobile phase.

scholarly journals HPLC method for the development and validation of busulfan in pharmaceutical formulation

2021 ◽  
Vol 6 (3) ◽  
pp. 136-142
Author(s):  
K Swamy Sekhar ◽  
Ch Venkata kishore ◽  
V Tejeswara Rao ◽  
K. Raghu Babu
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Detector Response ◽  
Control Analysis ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
System Controller

A validated HPLC method was developed for the determination of Busulfan (BUS) in pharmaceutical formulation.It is a new simple, accurate, precise and reproducible HPLC method has been developed for the estimation of Busulfan (1,4-butanediol dimethanesulfonate) in its inject able dosage.The method developed in High Performance Liquid Chromatographic method using suitable column (YMC Pack ODS-A (150 x 4.6) mm, 3µm). All the components of the system are controlled using SCL-10Avp System Controller. Data acquisition was done using LC Solutions software.The method was validated as per the ICH guidelines. Thus, the proposed HPLC method can be successfully applied for the routine quality control analysis of formulations. The method developed is simple and is better than the methods reported in the literature and the method is capable to give a good detector response, the recovery calculated was within the range of 98% to 102% of the specification limits.

Development and Validation of RP-HPLC Method for Simultaneous Estimation of Gatifloxacin and flurbiprofen Sodium in Eye Drops

2019 ◽  
Vol 9 (01) ◽  
pp. 83-88
Author(s):  
Pinkal Patel ◽  
Nalini Patel ◽  
Kinjal Parmar
Keyword(s):  
High Performance ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Eye Drops ◽  
Rp Hplc ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, selective and rapid reversed phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed and validated for the simultaneous analysis Gatifloxacin and flurbiprofen sodium in eye drops. The separation was carried out using a mobile phase consisting ACN: Buffer (pH 3.5) in the ratio of 55:45 v/v. The column used was Phenomenex luna ODS C18 (250mm X 4.6 mm i.d., 5 μm particle size) with flow rate of 1 ml / min using UV detection at 268 nm. The described method was linear over a concentration range of 2-12 μg/ml for both of Gatifloxacin and flurbiprofen sodium. The retention times of Gatifloxacin and flurbiprofen sodium were found to be 3.710 min. and 6.797 min respectively. Method was validated statistically and recovery studies were carried out. The proposed method has been applied successfully to the analysis of cited drugs either in pure form or in pharmaceutical formulations with good accuracy and precision. The method here in described can be employed for quality control and routine analysis of drugs in pharmaceutical formulations.

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF CLIDINIUM BROMIDE, CHLORDIAZEPOXIDE AND DICYCLOMINE HYDROCHLORIDE IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (4) ◽  
pp. 78-81
Author(s):  
Rajesh Sharma ◽  
◽  
Mukesh C. Sharma ◽  
Gaurav Vijaywargiya
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Water Ph ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic ◽  
Clidinium Bromide

A simple, specific, accurate reversed phase high performance liquid chromatographic method was developed for the simultaneous estimation of clidinium bromide, chlordiazepoxide and dicyclomine hydrochloride. Chromatographic separation of the three drugs was performed on a Chromatopak C-18 column (25 cm x 4.6 i.d. x 5µm) as the stationary phase with a mobile phase composed of 0.1 % triethylamine in water pH adjusted by 5 % o-phosphoric acid and acetonitrile in the ratio 30:70 at a flow rate of 0.8mL/min, Detection was carried out at 210 nm. The retention times of clidinium bromide, chlordiazepoxide and, dicyclomine hydrochloride were found to be 3.9 min, 5.4 min, and 6.8 min, respectively. The proposed method was validated for linearity, accuracy, precision, LOD and LOQ.

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