scholarly journals Development and validation of UV-Spectrophotometric and RP-HPLC method for simultaneous estimation of Metformin and Doxycycline in bulk and synthetic mixture

2021 ◽  
Vol 11 (4-S) ◽  
pp. 26-35
Author(s):  
Rajashree Mashru ◽  
Nirupa Koshti

A simple, rapid, sensitive, accurate and precise UV spectrophotometric and isocratic RP-HPLC method have been developed for simultaneous estimation of Metformin and Doxycycline in bulk and synthetic mixture. Spectrophotometric estimation was done by two methods. First method was Q-absorbance ratio method, where two wavelengths 236 nm (λmax of Metformin) and 248 nm (Iso-absorptive point) were used. The second method was first derivative method. In this method the zero-crossing point of Metformin was selected at 282 nm and for Doxycycline, it was 232 nm. The solvent used was methanol in both the above UV-spectrophotometric methods. Metformin and Doxycycline showed good linearity in the series of 1-9 µg/ml and 2-20 µg/ml respectively by both the two methods with an excellent correlation coefficient (r2≥0.998). In RP-HPLC method, the chromatographic separation was achieved on Luna Phenomenex C18 (150 mmХ6 mm, 5 µm) analytical column. A mixture of Acetonitrile: Phosphate buffer (50 mM): Triethylamine (TEA): Tetrahydrofuran (THF) (30:66:2:2) pH adjusted to 2.1 with orthophosphoric acid was used as the mobile phase, at a flow rate of 1 ml/min and at detector wavelength 248 nm. The retention time of Metformin and Doxycycline was found to be 3.561±0.0017 and 5.574±0.0131 minutes respectively. A linear response was observed over the concentration range 4-64 µg/ml of Metformin and 5-80 µg/ml of Doxycycline. All the three methods were validated in accordance to ICH guidelines for linearity, accuracy, precision, LOD and LOQ. The proposed methods were effectively utilized for the concurrent estimation of Metformin and Doxycycline in synthetic mixture. Keywords: Metformin, Doxycycline, Q-absorbance ratio method, First derivative method, RP-HPLC

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (09) ◽  
pp. 75-81
Author(s):  
Rakesh M Wani ◽  
Arun M Kashid ◽  
Amita Ghatge ◽  
Sumita Sahoo

The aim of the present work was to develop simple, precise and economic UV- spectrophotometric methods for the simultaneous estimation of aspirin and omeprazole in a laboratory sample. The absorbance maxima (λmax) for detection of aspirin and omeprazole were selected as 274 nm and 302 nm, respectively, for simultaneous equation method while wavelength range for detection of aspirin and omeprazole were selected as 270 nm - 276 nm and 300 nm - 305 nm, respectively for area under curve method. Absorbance ratio method uses the ratio of absorbances at two selected wavelengths, one which is an isoabsorptive point and other being the λ max of one of the two components. From the overlay spectra of two drugs, it is evident that aspirin and omeprazole show an isoabsorptive point at 238.6 nm. In zero crossing first derivative spectrophotometry, aspirin showed zero crossing point at 301nm and omeprazole showed zero crossing point at 274nm. Linearity for aspirin was between 25- 125 μg/mL and omeprazole it was 3-15 μg/mL. These methods were successfully applied for estimation of aspirin and omeprazole in the laboratory sample.


2020 ◽  
Vol 10 (5) ◽  
pp. 108-117
Author(s):  
Rajashree Mashru ◽  
Manthan Trivedi

The presented research work aims to develop and validate UV-Spectrophotometric as well as RP-HPLC methods for the simultaneous estimation of Beclomethasone Dipropionate (BDP) and Formoterol Fumarate Dihydrate (FFD). These methods offer a higher degree of sensitivity than the already present methods of analysis. By implementing advanced spectroscopic techniques such as Dual Wavelength Method and First Derivative Spectroscopy it is found that the sensitivity of the methods is increased. The linearity of both the methods was in the range of 10µg/ml to 50µg/ml for BDP and 1µg/ml to 5µg/ml for FFD, with an r2 value of 0.999 and 0.9988 respectively for Dual Wavelength Method and First Derivative Method. The LOD values of Dual Wavelength Method and First Derivative Method were found to be 0.127µg/ml and 0.016µg/ml respectively. A RP-HPLC Method has also been developed and validated for this combination having a linearity in range of 50µg/ml to 250µg/ml for BDP and 1.5µg/ml to 7.5µg/ml for FFD. The r2 value of BDP and FFD was found to be 0.9995 and 0.994. The application of this RP-HPLC Method may also be extended for the simultaneous estimation of a triple combination of Beclomethasone Dipropionate, Formoterol Fumarate and Glycopyrronium Bromide (GPB). Keywords: Beclomethasone, Formoterol, Glycopyrrolate, Dual-Wavelength-Method, First-Derivative, Spectroscopy, RP-HPLC


2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Shilan A. Omer ◽  
Nabil A. Fakhre

In this study, three simple and accurate spectrophotometric methods for simultaneous determination of pyriproxyfen and chlorothalonil residues in cucumbers and cabbages grown in experimental greenhouse were studied. The first method was based on the zero-crossing technique measurement for first and second derivative spectrophotometry. The second method was based on the first derivative of the ratio spectra. However, the third method was based on mean centering of ratio spectra. These procedures lack any previous separation steps. The calibration curves for three spectrophotometric methods are linear in the concentration range of 1–30 μg·mL−1 and 0.5–7 μg·mL−1 for pyriproxyfen and chlorothalonil successively. The recoveries ranged from 82.12–97.40% for pyriproxyfen and 81.51–97.04% for chlorothalonil with relative standard deviations less than 4.95% and 5.45% in all instances for pyriproxyfen and chlorothalonil, respectively. The results obtained from the proposed methods were compared statistically by using one-way ANOVA, and the results revealed there were no significant differences between ratio spectra and mean centering methods with the zero-crossing technique. The proposed methods are successfully applied for the simultaneous estimation of the residue of both pesticides in cucumber and cabbage samples.


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 100 (1) ◽  
pp. 38-44
Author(s):  
Kunjan Bodiwala ◽  
Shailesh Shah ◽  
Yogini Patel ◽  
Pintu Prajapati ◽  
Bhavin Marolia ◽  
...  

Abstract Two sensitive, accurate, and precise spectrophotometric methods have been developed and validated for the simultaneous estimation of ofloxacin (OFX), clotrimazole (CLZ), and lignocaine hydrochloride (LGN) in their combined dosage form (ear drops) without prior separation. The derivative ratio spectra method (method 1) includes the measurement of OFX and CLZ at zero-crossing points (ZCPs) of each other obtained from the ratio derivative spectra using standard LGN as a divisor, whereas the measurement of LGN at the ZCP of CLZ is obtained from the ratio derivative spectra using standard OFX as a divisor. The double divisor-ratio derivative method (method 2) includes the measurement of each drug at its amplitude in the double divisor-ratio spectra obtained using a standard mixture of the other two drugs as the divisor. Both methods were found to be linear (correlation coefficients of >0.996) over the ranges of 3–15, 10–50, and 20–100 μg/mL for OFX, CLZ, and LGN, respectively; precise (RSD of <2%); and accurate (recovery of >98%) for the estimation of each drug. The developed methods were successfully applied for the estimation of these drugs in a marketed ear-drop formulation. Excipients and other ingredients did not interfere with the estimation of these drugs. Both methods were statistically compared using the t-test.


2015 ◽  
Vol 5 (3) ◽  
pp. 175 ◽  
Author(s):  
Virani Paras ◽  
Sojitra Rajanit ◽  
Savaj Bhadresh ◽  
Raj Hashumati ◽  
Jain Vineet ◽  
...  

2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Monika L. Jadhav ◽  
Manoj V. Girase ◽  
Shripad K. Tidme ◽  
Manish S. Junagade

Two UV-spectrophotometric methods have been developed and validated for simultaneous estimation of valsartan and hydrochlorothiazide in a tablet dosage form. The first method employed solving of simultaneous equations based on the measurement of absorbance at two wavelengths, 249.4 nm and 272.6 nm, λmax for valsartan and hydrochlorothiazide, respectively. The second method was absorbance ratio method, which involves formation of Q-absorbance equation at 258.4 nm (isoabsorptive point) and also at 272.6 nm (λmax of hydrochlorothiazide). The methods were found to be linear between the range of 5–30 µg/mL for valsartan and 4–24 μg/mL for hydrochlorothiazide using 0.1 N NaOH as solvent. The mean percentage recovery was found to be 100.20% and 100.19% for the simultaneous equation method and 98.56% and 97.96% for the absorbance ratio method, for valsartan and hydrochlorothiazide, respectively, at three different levels of standard additions. The precision (intraday, interday) of methods was found within limits (RSD<2%). It could be concluded from the results obtained in the present investigation that the two methods for simultaneous estimation of valsartan and hydrochlorothiazide in tablet dosage form are simple, rapid, accurate, precise and economical and can be used, successfully, in the quality control of pharmaceutical formulations and other routine laboratory analysis.


Author(s):  
Mahesh Attimarad ◽  
Muhammad Shahzad Chohan ◽  
Abdulmalek Ahmed Balgoname

Simple, fast, and precise reversed-phase (RP)-high-performance liquid chromatography (HPLC) and two ecofriendly spectrophotometric methods were established and validated for the simultaneous determination of moxifloxacin HCl (MOX) and flavoxate HCl (FLX) in formulations. Chromatographic methods involve the separation of two analytes using an Agilent Zorbax SB C18 HPLC column (150 mm × 4.6 mm; 5 µm) and a mobile phase consisting of phosphate buffer (50 mM; pH 5): methanol: acetonitrile in a proportion of 50:20:30 v/v, respectively. Valsartan was used as an internal standard. Analytes were monitored by measuring the absorbance of elute at 299 nm for MOX and 250 nm for FLX and valsartan. Two environmentally friendly spectrophotometric (first derivative and ratio first derivative) methods were also developed using water as a solvent. For the derivative spectrophotometric determination of MOX and FLX, a zero-crossing technique was adopted. The wavelengths selected for MOX and FLX were −304.0 nm and −331.8 nm for the first derivative spectrophotometric method and 358.4 nm and −334.1 nm for the ratio first-derivative spectrophotometric method, respectively. All methods were successfully validated, as per the International Conference on Harmonization(ICH) guidelines, and all parameters were well within acceptable ranges. The proposed analytical methods were successfully utilized for the simultaneous estimation of MOX and FLX in formulations.


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