scholarly journals Development and Validation of RP-HPLC Method for the Simultaneous Estimation of Haloperidol and Trihexyphenidyl in API and Combined Tablet Dosage Form

Author(s):  
E. Amulya ◽  
N. Naveen Kumar ◽  
CH. Mounika ◽  
V. Kowmudi ◽  
N. Supriya ◽  
...  

A rapid and precise reverse phase high performance liquid chromatographic method has been developed for the validated of Trihexyphenidyl and Haloperidol, in its pure form as well as in tablet dosage form. Chromatography was carried out on a Altima C18 (4.6 x 150mm, 5μm) column using a mixture of Methanol: TEA Buffer pH 4.5: Acetonitrile (50:25:25) as the mobile phase at a flow rate of 1.0ml/min, the detection was carried out at 225 nm. The retention time of the Trihexyphenidyl and Haloperidol was 2.102, 3.537±0.02min respectively. The method produce linear responses in the concentration range of 15-75ppm of Trihexyphenidyland 37.5-187.5ppm of Haloperidol. The method precision for the determination of assay was below 2.0%RSD. The method is useful in the quality control of pharmaceutical formulations.

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (08) ◽  
pp. 12-16
Author(s):  
S Vidyadhara ◽  
◽  
L. S Reddyvalam ◽  
T. Koduri ◽  
P. K. Borra ◽  
...  

A simple, accurate, precise high-performance liquid chromatographic (HPLC) method has been developed and validated for the simultaneous determination of abacavir sulphate (ABA) and lamivudine (LAM) in combined dosage form. Separation was performed on a C18 column [Agilent ODS UG 5 column, 250 mm x 4.5 mm], with methanol: water (50:50 V/V) isocratic elution using a flow rate of 1mL/min. Good sensitivity was observed with UV detection at 277 nm. After method development, the interference of other active compounds and excipients, repeatability and linearity, were investigated. Retention times of LAM and ABA were found to be 3.3 and 6.3 min, respectively. The method was validated over the range from 2.5-12.5 μg/mL for LAM and 5-25 μg/mL for ABA with correlation coefficients of 0.9997 and 0.9996, respectively. This method was shown to be accurate, robust, selective, linear, and repeatable and can be successfully employed in routine quality control for the simultaneous analysis of ABA and LAM in tablets.


INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (05) ◽  
pp. 61-64
Author(s):  
A. L Rao ◽  
◽  
R. V Bhaskara

A reverse phase high performance liquid chromatographic method was developed and validated asper ICH guidelines for estimation of trandolapril and verapamil in combined tablet dosage form. Theseparation was obtained using a mobile phase consisting of acetonitrile and phosphate buffer adjustingpH to 3.0 in the ratio of 70:30 v/v and using Waters C18 (250 x 4.6 mm, 5 mcm) column maintained atambient temperature. The flow rate was 1.2 mL min-1 and UV detection was monitored at 215 nm. Theretention time (min) and linearity range (mcg mL-1) for trandolapril and verapamil were (5.12, 2.70) and(20-60, 20-60), respectively. The method validation results are within the acceptance criteria for precision,accuracy and linearity. The proposed method was found to be suitable for routine quality control ofmarketed formulation containing these APIs.


2020 ◽  
Vol 10 (5) ◽  
pp. 143-148
Author(s):  
T. Hanuman ◽  
T. Sivakkumar ◽  
S. Sridhar

A simple, specific and accurate reverse phase high performance liquid chromatographic method was developed for the simultaneous determination Sofosbuvir and Velpatasvirin pharmaceutical dosage form. The column used was Kromosil C18(150mm x 4.6 mm, 5mm)in isocratic mode, with mobile phase containing phosphate buffer andacetonitrile(70:30v/v). The buffer is prepared by adding 1.41gm of sodium dihyrogen ortho phosphate in a 1000ml of volumetric flask add about 900ml of milli-Q water added and degas to sonicate and finally make up the volume with water then pH adjusted to 3.5 with dil. orthophosphoric acid solution. The flow rate was 1.0ml/ min and effluents were monitored at 260 nm. The retention times of Sofosbuvir and Velpatasvirwere found to be 2.404min and 2.986 min, respectively. The linearity for Sofosbuvir and Velpatasvirwere in the range of 40-240µg/ml and 10-60 µg/ml respectively. The recoveries of Sofosbuvir and Velpatasvirwere found to be 99.64% and 99.25%, respectively. The proposed method was validated and successfully applied to the estimation of Sofosbuvir and Velpatasvirin combined tablet dosage forms. Keywords: Sofosbuvir, Velpatasvir, Validation, Buffer and ICH Guidelines.


2019 ◽  
Vol 9 (01) ◽  
pp. 83-88
Author(s):  
Pinkal Patel ◽  
Nalini Patel ◽  
Kinjal Parmar

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.


Author(s):  
Abrar Ahmed ◽  
Tayyaba Mahtab ◽  
Sumaiyya Saleem

Midostaurin is a multi-targeted protein kinase inhibitor that has been used for the treatment of acute myeloid leukemia.  Here, a rapid and precise reverse phase high-performance liquid chromatographic method has been developed for the validation of midostaurin, in its API form as well as in capsule dosage form. Chromatography was carried out on a X-Bridge C18 (4.6 x 250 mm, 5 µm) column using a mixture of methanol: water (75:25% v/v) as the mobile phase at a flow rate of 1.0 mL/min, the detection was carried out at 243nm and the retention time of the midostaurin was found to be 3.155. The method produce linear responses in the concentration range of 10-50 µg/mL of midostaurin. The method precision for the determination of assay was below 2.0 % RSD. The LOD and LOQ values obtained were 1.2 µg/mL and 3.8 µg/mL respectively. There were no significant changes observed upon changing chromatographic conditions indicating the method to be robust. Therefore this validated method can be useful in the quality control of bulk and pharmaceutical formulations of midostaurin. 


INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (4) ◽  
pp. 78-81
Author(s):  
Rajesh Sharma ◽  
◽  
Mukesh C. Sharma ◽  
Gaurav Vijaywargiya

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.


2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
Patel Bhaumik ◽  
Gopani Mehul ◽  
Vikani Kartik ◽  
Patel Rashmin ◽  
Patel Mrunali

This paper describes validated reverse phase high-performance liquid chromatographic (RP-HPLC) method for simultaneous estimation of trihexyphenidyl hydrochloride (THP) and risperidone (RSP) in the pure powder form and in combined tablet dosage form. The HPLC separation was achieved on a core shell C18 (100 mm length × 4.6 mm, 2.6 μm particle size) using methanol : ammonium acetate buffer 1% (85 : 15 v/v; pH-6.5) as mobile phase and delivered at flow rate of 0.8 mL/min. The calibration plot showed good linear relationship with r2 = 0.997 ± 0.001 for THP and r2 = 0.998 ± 0.001 for RSP in concentration range of 50–175 μg/mL and 50–175 μg/mL, respectively. LOD and LOQ were found to be 0.40 and 1.29 μg/mL for THP and 1.24 and 3.92 μg/mL for RSP. Assay of THP and RSP was found to be 100.16 ± 0.03% and 99.83 ± 0.02%, respectively. THP and RSP were subjected to different stress conditions (acidic, basic, oxidative, thermal, and photolytic degradation). The degraded product peaks were well resolved from the pure drug peak. The method was successfully validated as per the ICH guidelines. The developed RP-HPLC method was successfully applied for the estimation of THP and RSP in tablet dosage form.


INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (01) ◽  
pp. 50-53
Author(s):  
S. B. Jadhav ◽  
◽  
V. V Kunjir ◽  
S. K. Kupkar ◽  
P. D. Chaudhari

A simple, specific, accurate and precise reverse phase high performance liquid chromatographic method was developed for the simultaneous estimation of olmesartan medoxomil and metoprolol succinate in tablet dosage form. A Phenomenex-C18, 5 mcm column 250 mm 4.6 mm in gradient mode, with mobile phase containing phosphate buffer, acetonitrile and methanol in proportion of 65:35 v/v, pH 5.5 adjusted with orthophosphoric acid were used. The flow rate was 1 mL/min, and effluent was monitored at 254 nm.The retention time of olmesartan medoxomil and metoprolol succinate were 8.02 and 5.36 min respectively, and the resolution factor was 9.0. Linearity range for olmesartan medoxomil and metoprolol succinate was 5-30 mcg mL-1 and 5-70 mcg mL-1 respectively. The proposed method is accurate, precise,specific and rapid for simultaneous estimation of olmesartan medoxomil and metoprolol succinate in tablet dosage form.


INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (01) ◽  
pp. 76-78
Author(s):  
Kailasa Mangasree ◽  
◽  
Biswabara Roy ◽  
Harunrasheed Shaik ◽  
Manjunath S. Yalagatti ◽  
...  

A reverse phase high performance liquid chromatographic method was developed for simultaneous estimation of gemcitabine and clarithromycin in bulk and tablet dosage form. The method was developed by using acetonitrile: methanol: 50 mM sodium acetate buffer (adjusted to pH-3 with orthophosphoric acid (40:40:20) as a mobile phase at the flow rate of 1mL/min. The retention time was found to be 2.365 and 5.999 minutes, respectively. The method showed linearity in the concentration range 10-50 µg/mL in respect of both drugs. The % RSD was less than 0.4% for gemcitabine and 0.2% for clarithromycin. Mean percentage recovery was found to be 99.63 and 99.69 for gemcitabine and clarithromycin. The tailing factor for gemcitabine and clarithromycin was not less than 0.9 and not more than 1.4 during the robustness study. The average percentage assay was calculated and found to be 99.83 for gemcitabine and 98.89 for charithromycin. The limit of detection and quantification for gemcitabine was found to be 0.41 and 1.79 µg/mL. For Clarithromycin, the value was 0.58 and 1.37 µg/mL respectively.


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