QBD ASSISTED RP-HPLC METHOD FOR IDENTIFICATION OF TERAZOSIN IN BULK DRUG AND PHARMACEUTICAL SAMPLE

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (03) ◽  
pp. 19-26
Author(s):  
C. Dhal ◽  
◽  
D. Rajput ◽  
V. Tiwari ◽  
A. Teotia ◽  
...  

Reversed Phase High Performance Liquid Chromatographic (RP-HPLC) proves to be a convenient and reliable technique for the identification of various compounds, such as pharmaceutical drugs of chemical as well as phyto origin, food compounds and others. Analytical method for the estimation of alpha-1 antagonist terazosin, a potent anti-hypertensive agent for enlarged prostate, was developed, optimized for the best fit condition using statistical software Minitab and validated as per International Conference on Harmonization (ICH) Q2 (R1) guidelines. Partitioning of the desired molecule was achieved on Agilent Zorbax C18 column with dimensions of 250 mm X 4.6 mm and a particle size 5μm against mobile phase containing acetate buffer adjusted to pH 6.0 and acetonitrile (ACN) in a ratio 30:70 (V/V), run isocratically for sufficient time. The linear model was established between 50 – 250 ppm with a regression coefficient (r2) of 0.9971 and with detection (LOD) and quantification limit (LOQ) of 17.754 ppm and 53.802 ppm, respectively. The method was precise, accurate, robust and able to distinguish between the adduct generated during forced degradation studies.

Author(s):  
T Hemant Kumar ◽  
CH. ASHA ◽  
D. GOWRI SANKAR

Objective: To develop and validate a simple, specific, accurate, precise and sensitive reverse phase high performance liquid chromatographic (RP-HPLC) method with forced degradation studies for the simultaneous estimation of amlodipine besylate and irbesartan in the pharmaceutical formulation. Methods: The chromatographic separation of the two drugs were achieved using Enable C 18G column (250 ×4.6 mm; 5 µm) in isocratic mode with mobile phase consisting of sodium acetate buffer (pH 4.0) and acetonitrile (30:70, % v/v) with a flow rate of 0.6 ml/min. Ultraviolet(UV) detection was carried out at 238 nm. The proposed method was validated for linearity, range, accuracy, precision, robustness, limit of detection (LOD) and limit of quantification (LOQ). The tablet formulation was subjected to stress conditions of degradation including acidic, alkaline, oxidative, thermal and photolysis. Results: The retention time for amlodipine besylate and irbesartan were found to be 5.512 and 6.321 min respectively. Linearity was observed over a concentration range 4-32 µg/ml for amlodipine besylate (r2 =0.9999) and 10-70 µg/ml for Irbesartan (r2 =0.9998). The % relative standard deviation (RSD) for Intraday and Interday precision was found to be 0.436 and 0.699 for amlodipine besylate and 0.435 and 0.30 for irbesartan. Amlodipine besylate shown stability towards acidic and thermal whereas in basic, oxidative and photolytic it shown less stability in which it degraded to more extent. Irbesartan shown stability towards thermal conditions whereas in remaining conditions it degrades to more extent especially in oxidative conditions. Conclusion: The developed reverse phase high performance liquid chromatographic (RP-HPLC) method was also found to be simple, precise and sensitive for the simultaneous determination of amlodipine besylate and irbesartan in the tablet dosage form.


2008 ◽  
Vol 91 (5) ◽  
pp. 1070-1074 ◽  
Author(s):  
Arun M Prajapati ◽  
Satish A Patel ◽  
Natvarlal J Patel ◽  
Dipti B Patel ◽  
Sejal K Patel

Abstract This research paper describes validated reversed-phase high-performance column liquid chromatographic (RP-HPLC) and first-derivative UV spectrophotometric methods for the estimation of voriconazole (VOR) in oral suspension powder. The RP-HPLC separation was achieved on Phenomenex C18 column (250 4.6 mm id, 5 m particle size) using wateracetonitrile (40 + 60, v/v; pH adjusted to 4.5 0.02 with acetic acid) as the mobile phase at a flow rate of 1.4 mL/min and ambient temperature. Quantification was achieved with photodiode array detection at 255 nm over the concentration range of 0.11 g/mL with mean recovery of 99.49 0.83 for VOR by the RP-HPLC method. Quantification was achieved with UV detection at 266 nm over the concentration range of 820 g/mL with mean recovery of 99.74 0.664 for VOR by the first-derivative UV spectrophotometric method. These methods are simple, precise, and sensitive, and they are applicable for the determination of VOR in oral suspension powder.


2017 ◽  
Vol 15 (2) ◽  
pp. 187-194 ◽  
Author(s):  
Md Shahadat Hossain ◽  
Md Samiul Islam ◽  
Subrata Bhadra ◽  
Abu Shara Shamsur Rouf

Highly nutritious dairy products are ingested regularly by all ages of population. Adulteration of dairy products to enhance the inherent stability and acceptability to common consumers by different harmful and toxic ingredients like formalin, an unpermitted preservative, has been a burning issue in Bangladesh over the last few years. The aim of this paper was to analyze the concentration of formaldehyde in dairy products most commonly sold in Bangladeshi markets by a validated reversed phase high performance liquid chromatographic (RP-HPLC) method to reveal the on-going alarming scenario in a scientific way. After pre-derivatization with 2,4- dinitrophenylhydrazine, formaldehyde was detected at 345 nm using a C18 column with acetonitrile and water (45:55) as mobile phase at a flow rate of 2.0ml/min. The validated method has been applied to 41 marketed dairy products, including pasteurized milk, UHT milk, banana- mango- and chocolate-milk, flavored yoghurt, lassi, buttermilk, and skimmed milk. However, no formaldehyde was detected among the tested dairy products.Dhaka Univ. J. Pharm. Sci. 15(2): 187-194, 2016 (December)


2010 ◽  
Vol 7 (s1) ◽  
pp. S299-S313 ◽  
Author(s):  
P. Shetti ◽  
A. Venkatachalam

A new, simple, precise, rapid, selective and stability indicating reversed-phase high performance liquid chromatographic (HPLC) method has been developed and validated for simultaneous quantification of trihexyphenidyl hydrochloride, trifluoperazine hydrochloride and chlorpromazine hydrochloride from combined tablet formulation. The method is based on reverse-phase using C-18 (250×4.6) mm, 5 μm particle size column. The separation is achieved using isocratic elution by methanol and ammonium acetate buffer (1% w/v, pH 6.5) in the ratio of 85:15 v/v, pumped at flow rate 1.0 mL/min and UV detection at 215 nm. The column is maintained at 30 °C through out the analysis. This method gives baseline resolution. The total run time is 15 min. Stability indicating capability is established buy forced degradation experiment. The method is validated for specificity, accuracy, precision and linearity as per International conference of harmonisation (ICH). The method is accurate and linear for quantification of trihexyphenidyl hydrochloride, trifluoperazine hydrochloride and Chlorpromazine hydrochloride between 5 - 15 μg/mL, 12.5- 37.5 μg/mL and 62.5 - 187.5 μg/mL respectively.


2012 ◽  
Vol 10 (2) ◽  
pp. 67-70
Author(s):  
Abdullah Al Masud ◽  
Mohammad Saydur Rahman ◽  
Towfika Islam ◽  
Saki Sultana ◽  
Moynul Hasan ◽  
...  

A simple, reproducible and efficient reversed phase high performance liquid chromatographic (RPHPLC) method has been developed for the estimation of a recently approved anti allergic drug, amlexanox in oral paste dosage form. The separations were carried out on a Zorbax Eclipse XBD, C18 column (150 x 4.6 mm; 5?m) at a flow rate of 1.50 ml/min. by using mobile phase comprising of mixed buffer (pH adjusted to 6.50) and methanol (50:50 v/v). The injection volume was 10 ?l and the peaks were detected at 244 nm. The linear dynamic range found to be in the concentration range of 15-35 ?g/ml and coefficient of correlation was found to be 0.999. The %RSD value was below 2.0 for intra-day and inter-day precision which indicated that the method was highly precise. The LOD (Limit of detection) and LOQ (Limit of quantitation) were found to be 3.8 ng/ml and 12.5 ng/ml, respectively which revealed that the method was highly sensitive. The percentage recovery of amlexanox ranged from 99.31 to 99.75%, indicating the accuracy of the method and absence of interference from the excipients present in the formulation. The proposed method was simple, fast, accurate and reproducible and hence can be applied for routine quality control operations of amlexanox in oral paste dosage form. Key words: Amlexanox, Anti allergic, RP-HPLC, LOD, LOQ. DOI: http://dx.doi.org/10.3329/dujps.v10i2.11782 Dhaka Univ. J. Pharm. Sci. 10(2): 67-70, 2011 (December)


Author(s):  
Zahid Zaheer ◽  
Sarfaraz Khan ◽  
Mohammad Sadeque ◽  
Hundekari G. I. ◽  
Rana Zainuddin

A simple, reproducible and efficient reverse phase high performance liquid chromatographic method was developed for Lisinopril in bulk drug and formulation. A column having 150 × 4.6 mm in isocratic mode with mobile phase containing acetonitrile: phosphate buffer (70:30; adjusted to pH 3.0) was used. The flow rate was 0.8 ml/min and effluent was monitored at 216 nm. The retention time (min) and linearity range (μg/ml) for Lisinopril was (1.510) and (10-35). The developed method was found to be accurate, precise and selective for determination of Lisinopril in bulk and formulation.


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.


2011 ◽  
Vol 8 (4) ◽  
pp. 1958-1964 ◽  
Author(s):  
H. R. Prajapati ◽  
P. N. Raveshiya ◽  
J. M. Prajapati

A reversed phase high performance liquid chromatographic (RP–HPLC) method was developed and subsequently validated for the determination of atomoxetine hydrochloride in bulk and pharmaceutical formulation. The separation was done by a PerkinElmer Brownlee analytical C8 column (260 mm x 4.6 mm, 5 µm) using methanol: 50 mM KH2PO2buffer (PH adjusted to 6.8 with 0.1 M NaOH), 80:20 v/v as an eluent. UV detection was performed at 270 nm at a flow rate 1.0 mL/min. The validation of the method was performed, and specificity, reproducibility, precision accuracy and ruggedness were confirmed. The correlation coefficient was found to be 0.997 for atomoxetine hydrochloride. The recovery was in the range of 99.94 to 100.98% and limit of quantification was found to be 5.707 µg/mL. The method is simple, rapid, selective and economical too and can be used for the routine analysis of drug in pharmaceutical formulations.


2020 ◽  
Vol 13 (3) ◽  
pp. 206-216
Author(s):  
Madhusudan Bhoir ◽  
Nutan Rao

The objective of the study was to develop and validate a novel, stability indicating, simple, rapid, accurate, precise and isocratic reverse-phase high-performance liquid chromatographic (RP-HPLC) method for simultaneous estimation of benserazide HCl and levodopa in a marketed formulation. Chromatographic separation was achieved by using C18 Cosmosil 4.6 × 250 mm column with a mixture of phosphate buffer pH 2 and acetonitrile in proportion of 95:5 as mobile phase at a flow rate of 1.0 ml/min and column temperature 25°C. The detection was carried out at 210 nm using UV detector. The retention time for benserazide and levodopa was found to be 3.1 minutes and 6.6 minutes respectively and recoveries from tablet were between 98 and 102 %.


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