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Papers by Sunitha Gurrala

Journal of chromatographic science, 2021

New analytical quality by design-oriented HPLC method with multiple response optimization (Derrin... more New analytical quality by design-oriented HPLC method with multiple response optimization (Derringer's desirability function) was demonstrated for simultaneous analysis of three antidiabetic drugs (metformin hydrochloride/empagliflozin/linagliptin) in a fixed-dose combination. Central composite design was employed for systematic optimization of critical method parameters, namely, % organic phase (X1), aqueous phase pH (X2) and flow rate (X3) while resolution, capacity factor and theoretical plate number as critical analytical attributes. Effective chromatographic separation of title analytes was accomplished on Std. Discovery C18 column at 30°C with mobile phase comprising acetonitrile: phosphate buffer pH 5 (38:62% v/v), pumped at a flow rate of 1 mL/min by isocratic elution pattern and UV detection at 222 nm. The model is rectilinear in the range of 1.0-200, 0.2-40 and 0.1-20 μg/mL at retention times of 3.04, 3.93 and 5.99 min for metformin, empagliflozin and linagliptin, resp...

Future Journal of Pharmaceutical Sciences, 2021

Analytical quality by design driven HPLC method has been optimized for simultaneous estimation of... more Analytical quality by design driven HPLC method has been optimized for simultaneous estimation of dapagliflozin and saxagliptin in pharmaceutical dosage form. Response surface methodology was employed for optimization of experimental conditions using three factors such as organic phase (%), pH of aqueous phase, and flow rate of mobile phase. Virtuous separation of analytes was achieved with mobile phase consisted of acetonitrile: phosphate buffer, pH 5.8 (26:74% v/v) with flow rate 0.96 mL/min using SPOLAR C18 column (250 × 4.6 mm, 5 μ) with run time 6 min and UV detection at 236 nm. Retention time for dapagliflozin and saxagliptin were found to be 3.5 and 5.0 min, respectively. Method was validated as per ICH guidelines. The plot between peak area vs concentration for dapagliflozin and saxagliptin were rectilinear in the range of 0.2-300 μg/mL and 0.1-150 μg/mL respectively with detection and quantification limits were 0.061 and 0.18 μg/mL for dapagliflozin and 0.014 and 0.043 μg/m...

The Turkish Journal of Pharmaceutical Sciences

Amaç: Bu çalışmanın amacı tamsulosin hidroklorür ve solifenasin süksinatın aynı anda miktar tayin... more Amaç: Bu çalışmanın amacı tamsulosin hidroklorür ve solifenasin süksinatın aynı anda miktar tayininin yapılabilmesi için basit bir senkronize spektroflorimetri yöntemi geliştirmek ve valide etmektir. Gereç ve Yöntemler: Bahsedilen analitlerin aynı anda miktar tayinlerinin yapılabilmesi için birinci türev senkronize spektroflorimetri yöntemi kullanılmıştır. Tamsulosin hidroklorür 322 nm de ölçüm yapılarak (bu dalga boyu solifenasin süksinatın sıfır kesim noktasıdır) solifenasin süksinat ise 570 nm de ölçüm yapılarak (bu dalga boyu tamsulosin hidroklorürün sıfır kesim noktasıdır) miktar tayinleri gerçekleştirilmiştir. Bulgular: Kalibrasyon eğrileri tamsulosin hidroklorür için 2-10 μg/mL, solifenasin süksinat için ise 30-150 μg/mL konsantrasyon aralığında hazırlanmıştır. Geliştirilen yöntemle; ICH kılavuzlarına göre hesaplanan doğrusallık, seçicilik, doğruluk, kesinlik ve LOD ve LOQ değerleri kullanılarak başarılı sonuçlar elde edilmiştir. Önerilen yöntemle yapılan analiz sonuçları ticari formülasyon içerisinde tamsulosin hidroklorürün %95.0 solifenasin süksinatın ise %103.5 oranında bulunduğunu göstermiştir. Bu sonuçlar preparatın üzerinde belirtilen değerler ile iyi bir uygunluk göstermektedir. Sonuç: Önerilen analitik yöntemin tablet dozaj formlarında tamsulosin hidroklorür ve solifenasin süksinatın rutin kontrol analizlerinde kullanılabileceği anlaşılmıştır. Anahtar kelimeler: Tamsulosin hidroklorür, solifenasin süksinat, senkronize spektroflorimetri, yöntem validasyonu Objectives: The present study was undertaken with the objective to develop and validate a simple spectrofluorimetric method for the simultaneous quantification of tamsulosin hydrochloride and solifenacin succinate. Materials and Methods: First-derivative synchronous spectrofluorimetry was attempted for the simultaneous quantification of the analytes. Tamsulosin hydrochloride was quantified at a wavelength of 322 nm (zero-crossing wavelength point of solifenacin succinate) and solifenacin succinate was measured at 570 nm (zero-crossing wavelength point of tamsulosin hydrochloride). Results: Calibration plots were constructed over the concentration range of 2-10 μg/mL for tamsulosin hydrochloride and 30-150 μg/mL for solifenacin succinate. The method gave satisfactory results when it is validated for linearity, specificity, accuracy, precision, LOD and LOQ as per the ICH guidelines. The assay values in the commercial formulation were found to be in the percentage range of 95.0 for tamsulosin hydrochloride and 103.5 for solifenacin succinate by the proposed method. These results were well in agreement with their label claim. Conclusion: The proposed synchronous analytical method can be employed for routine quality control analysis of tamsulosin hydrochloride/ solifenacin succinate in tablet dose forms.

INDIAN DRUGS

A simple and sensitive spectrofluorimetric method has been developed for the estimation of mesala... more A simple and sensitive spectrofluorimetric method has been developed for the estimation of mesalamine (MES). Linearity was obeyed in the range of 0.1-2.5 µg/mL in distilled water as solvent at an emission wavelength (λem) of 501 nm after excitation (λex) at 332 nm, with a good correlation coefficient of 0.999. The limit of detection and limit of quantification for this method were 0.05 and 0.1 µg/mL, respectively. The developed method was statistically validated as per ICH guidelines. The percentage relative standard deviation values were found to be less than 2 for accuracy and precision studies. The assay results obtained were in good agreement with the labeled amounts of the marketed formulations. This validated method was extended to study the degradation behavior of mesalamine in various conditions such as acid, alkaline, oxidative, thermal, and UV effects. Although there was no degradation observed in oxidative, thermal, UV effect, 41.9 % and 11.6 % amount was degraded in acid...

Turkish Journal of Pharmaceutical Sciences

Future Journal of Pharmaceutical Sciences

Background A simple and sensitive spectrophotometric method was developed for the quantitative me... more Background A simple and sensitive spectrophotometric method was developed for the quantitative measurement of dolutegravir in pure form and pharmaceutical formulation. The present method was based on redox reaction between dolutegravir and ferric chloride, which upon complexation with 1,10-phenanthroline formed an orange-colored complex that showed absorption maximum at 520.0 nm. Results The developed method obeyed linearity in the concentration range of 40.00–140.00 μg/mL. The method was also validated as per International Council for Harmonization guidelines and the results were within acceptance values. The validated method was employed for the determination of dolutegravir in pharmaceutical dosage form and the percentage assay value was found to be 102.5, which is in agreement with its label claimed. Conclusion The developed redox-based colorimetric method could be used in the routine quality control analysis of dolutegravir present in various pharmaceutical dosage forms.

Journal of Applied Pharmacy

Purpose: In this present work a simple, rapid, specific and highly sensitive spectrofluorimetric ... more Purpose: In this present work a simple, rapid, specific and highly sensitive spectrofluorimetric method was developed and validated for the quantification of tapentadol HCl bulk drug and pharmaceutical dosage forms and proposed method was also applied to study of forced degradation and in-vitro dissolution studies. Materials and Methods: The fluorescence intensity of tapentadol HCl in distilled water was measured at emission wavelength 592 nm after excitation at 272 nm by using a Shimadzu (Japan) RF-5301 PC spectrofluorophotometer. A linear relationship was found between fluorescence intensity and concentration in the range of 1-6 µg/mL with a good correlation coefficient-0.999. Results: The detection and quantification limits were found to be 23.01 and 76.72 ng/mL, respectively. The proposed method was applied for quantification of tapentadol HCl in tablets, with percentage recovery of 99.95-101.45% and percentage RSD values were found to be less than 2 for accuracy and precision studies. Statistical analysis of the results revealed high accuracy and good precision. Conclusion: The suggested procedures could be used for the determination of tapentadol HCl in drug substance and drug products as well as in presence of its degradation products.

Journal of Applied Pharmacy

A reverse phase stability indicating HPLC method was developed for the analysis of efavirenz bulk... more A reverse phase stability indicating HPLC method was developed for the analysis of efavirenz bulk and pharmaceutical formulations. The developed method was also utilized for in-vitro dissolution studies of efavirenz formulations. Acetonitrile and acetate buffer pH 3.4 was the mobile phase (75:25% v/v), with retention time of 4.007 min at a flow rate of 1.5 mL/min detected at 292 nm wavelength. Linear regression analysis calibration plot showed an excellent linearity between response and concentration in the range of 50-300 μgmL-1. The regression coefficient was 0.999 and the linear regression equation was y = 7780x+11159. Limits of detection (LOD) and quantification (LOQ) were 0.238 and 0.793 μgmL-1 respectively. The method was validated for accuracy, precision, specificity, robustness, detection and quantification limits, in accordance with ICH guidelines. The specificity of the method was ascertained by forced degradation studies by acid, alkali hydrolysis, oxidation and thermal degradation methods. The degraded products were well resolved from the analysis peak with significant differences at their retention time values. Wide linearity range, sensitivity, accuracy, short retention time and simple mobile phase indicate the method is suitable for routine quantification of efavirenz with high precision and accuracy.

Indian Journal of Pharmaceutical Education and Research

Aim: Current work entails the analytical quality by design (AQbD) based robust HPLC method for re... more Aim: Current work entails the analytical quality by design (AQbD) based robust HPLC method for real-time analysis of canagliflozin and metformin. Different pKa values of two drugs made their chromatographic separation critical. Materials and Methods: The critical method parameters were systematically optimized using factorial experimental design (central composite design) and contours were generated as a function of significant variables when analyzed in the modeling software. The method operable design region that control the variation in response is obtained from contour plot and verified experimentally. Results: Effective chromatographic separation of title analytes was accomplished on SPOLAR C 18 (250 x 4.6 mm, 5µ) column at 25°C with mobile phase comprising of phosphate buffer, pH 6.0 and acetonitrile (55:45 % v/v), pumped at a flow rate of 0.8 mL/ min by isocratic elution pattern and UV detection at 254 nm. The linear model was established in the range of 50-300 and 5-30 and µg/mL at retention times of 3.24 and 10.77 min for metformin and canagliflozin, respectively. Conclusion: Method obeyed all validation parameters of ICH Q2 (R1) guidelines and able to discriminate the Adduct generated upon drug degradation. The proposed method was pertinent for assay drugs and extended to quantify the drugs in prevalence of biological matrix.

Turkish Journal of Pharmaceutical Sciences

Prazikuantel miktar tayini için basit, hızlı, spesifik ve yüksek duyarlılığa sahip, çevre dostu s... more Prazikuantel miktar tayini için basit, hızlı, spesifik ve yüksek duyarlılığa sahip, çevre dostu spektrofluorimetrik bir yöntem geliştirilmiştir. Gereç ve Yöntemler: Prazikuantel konsantrasyonu ile floresan yoğunluğu arasında, 1-20 μg/mL aralığında su içinde, 286 nm emisyon ve 263 nm eksitasyon dalga boyunda, iyi bir korelasyon katsayısı (0.999) olan doğrusal bir ilişki bulundu. Bulgular: Önerilen yöntem Uluslararası Uyumlaştırma Konferansı yönergelerine göre doğrulanmıştır ve sonuçların istatistiksel analizi, 2'den düşük bağıl standart sapma değerleri ile yüksek doğruluk ve hassasiyet göstermiştir. Saptama ve miktar limitleri sırasıyla 0.27 ve 0.81 μg/mL'dir. Önerilen yöntem, ilacın stabilitesini ve asidik, alkali ve oksidatif koşullar varlığında bozunma kinetiklerini araştırmak için genişletilmiştir. Sonuç: Yöntem, prazikuantel tablet formülasyonunun in vitro çözünme çalışmaları için kullanılmıştır. Önerilen prosedürler, prazikuantelin ilaç maddesi ve ilaç ürünlerinde ve degradasyon ürünlerinin varlığının değerlendirilmesi için kullanılabilir. Anahtar kelimeler: Prazikuantel, eksitasyon dalga boyu-263 nm, emisyon dalga boyu-286 nm, çözünme, zorla bozunma Objectives: A simple, rapid, specific, and highly sensitive ecofriendly spectrofluorimetric method has been developed for the quantification of praziquantel. Materials and Methods: A linear relationship was found between fluorescence intensity and praziquantel concentration in the range of 1-20 μg/mL in water at emission wavelength of 286 nm after excitation wavelength at 263 nm with a good correlation coefficient (0.999). Results: The proposed method was validated according to International Conference on Harmonization guidelines and statistical analysis of the results revealed high accuracy and good precision with the percentage relative standard deviation values less than 2. The detection and quantification limits were 0.27 and 0.81 μg/mL, respectively. The proposed method was extended to investigate the stability of the drug and its degradation kinetics in the presence of acidic, alkaline, and oxidative conditions. Conclusion: The method was utilized for in vitro dissolution studies of praziquantel tablet formulation. The suggested procedures could be used for the assessment of praziquantel in drug substance and drug products as well as in the presence of its degradation products.

Turkish Journal of Pharmaceutical Sciences

Amaç: Günümüzde, çeşitli dozaj formlarında etkin madde kombinasyonlarına rağbet edilmektedir, anc... more Amaç: Günümüzde, çeşitli dozaj formlarında etkin madde kombinasyonlarına rağbet edilmektedir, ancak bunlardaki etkin maddeleri tayin etmek için farmakope yöntemleri bulunmamaktadır. Bu çalışmada, kombine dozaj formunun analizi için kalite kontrol testini sadeleştirmek amacıyla tek bir çözünme testi yöntemi tercih edilmiştir. Gereç ve Yöntemler: Suda çözünürlüğü sınırlı olan ilacın çözünme yöntemi için geliştirilen çözünme ortamı in vivo davranışlarının kalitatif tahmininde biyouyumlu bir yöntem olarak kullanışlı bulunmuştur. Bulgular: Atorvastatin ve fenofibrat içeren kapsüllerde çözünme profilleri, 37±0.5°C'de, 50 rpm ve 900 mL ortam içinde bir palet tipi Amerikan Farmakopesi çözünme cihazı ile değerlendirildi. En iyi ortam, 900 mL %0.5 a/h sodyum lauril sülfattır. Piyasadaki tabletler için kümülatif % çözünme, 45 dakika içinde %85'ten fazla olmuştur. Önerilen çözünme testi koşulları ayırt edici bir güce sahiptir, farklılık faktörü (f 1) değerleri düşüktür (%12-16) ve benzerlik (f 2) faktör değerleri de düşüktür (%45-48). Bu nedenle, %0.5 w/v sodyum lauril sülfat çözeltisinin kullanımı uygundur. Objectives: Nowadays, the market is flooded with combinations of drugs in various dosage forms, but there is a lack of official methods to quantify them. A single dissolution test method for the analysis of combined dosage form is preferred for simplification of quality control testing. Materials and Methods: If the developed dissolution medium mimics the biorelevant and discriminating dissolution procedure for drug products with limited drug aqueous solubility it is a useful tool for qualitative forecasting of the in vivo behavior of formulations. Results: Dissolution profiles were evaluated for atorvastatin and fenofibrate in capsules, using a paddle-type United States Pharmacopeia dissolution apparatus in 900 mL of medium at 50 rpm and 37±0.5°C. The best medium was 900 mL of 0.5% w/v sodium lauryl sulfate. The cumulative % dissolution was more than 85% within 45 min for marketed tablets. The proposed dissolution test conditions have discriminative power, dissimilarity factor (f 1) values are low (12-16%), and similarity (f 2) factor values are also low (45-48%). Hence the use of 0.5% w/v sodium lauryl sulfate solution is justified. Conclusion: The dissolution method was validated (% relative standard deviation <2). To quantify both drugs simultaneously, a second derivative spectrophotometric method was established (λ max 281 nm and 296 nm, respectively, for atorvastatin and fenofibrate) in acetate buffer, pH 2.8 solution.

Turkish Journal of Pharmaceutical Sciences

spectrophotometric methods have been developed and validated for quantification of Lornoxicam (LO... more spectrophotometric methods have been developed and validated for quantification of Lornoxicam (LOR) and Mesalamine (MES) drugs in pure form and in pharmaceutical formulations. MATERIALS AND METHODS: Shimadzu Double-beam UV-Visible Spectrophotometer 1800 having spectral bandwidth of 0.1 nm with wavelength accuracy ±0.1 nm and a pair of 1 cm path length matched quartz cells were used to measure absorbance of the resulting solution. Method (I) is used for the quantification of LOR which is based on the measurement of absorbance of bluish green coloured chromogen complex at 760 nm which is formed by reaction of LOR with ferric chloride and potassium ferricyanide (redox technique). Method (II) is used for the quantification of MES that is based on measurement of absorbance of yellow coloured chromogen at 400 nm which is formed by the condensation reaction of the primary amino group of MES with salicylaldehyde reagent (SA) (Schiff base formation). RESULTS: Both the methods obeyed Beer's law in concentration range of 0.5-4.5 μg/mLand 0.2-1.7 μg/mL with good correlation coefficients of 0.9974 and 0.998 for Methods (I) and (II) respectively. CONCLUSION: The developed method is simple, sensitive, specific which is validated statistically as per ICH guidelines and can be used in routine analysis of LOR and MES pharmaceutical dosage forms.

International Journal of Research in Pharmaceutical and Biomedical Sciences

____________________________________________________________________________________ A simple, ra... more ____________________________________________________________________________________ A simple, rapid accurate and stability indicating RP-HPLC method was developed for the determination of Capecitabine in pure and tablet dosage form. The method showed a linear response for concentrations in the range of 70-120 µg/ml using 0.05M phosphate buffer (p H 3.0 ± 0.05) buffer and acetonitrile (50:50 % w/v) as the mobile phase with detection at 240 nm and a flow rate of 1 mL/min and retention time 4.108 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, forced degradation, solution stability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from recovery studies was found to be less than 1. The specificity of the method was ascertained by forced degradation studies by acid, alkali hydrolysis, oxidation and thermal degradation. The degraded products were well resolved from th...

Asian Journal of Pharmaceutical and Clinical Research

Dissolution process is considered as an important in vitro tool for evaluating the bioequivalence... more Dissolution process is considered as an important in vitro tool for evaluating the bioequivalence of products. Such a method, if properly mimic the in vivo conditions, it would surrogate the in vivo studies. Bioequivalence problems arise in class-II and class-IV categories of Biopharmaceutical Classification of Drugs (BCS). Efavirenz (BCS Class II drug) is used in active anti retroviral therapy. Saturation solubility of efavirenz bulk drug was evaluated in various surfactant media, pH solutions and bio-relevant media. We optimized the dissolution conditions for efavirenz with 900 ml of simulated gastric fluid with 0.25% w/v sodium lauryl sulphate (SGF-0.25% w/v SLS) as discriminating and bio-relevant dissolution medium at 50 rpm for 45 min (5 min time interval) with USP apparatus II. The optimized media contained a less amount of SLS (0.25% w/v) in SGF compared with 1% and 2% SLS concentration stated in the official monographs (IP, BP, USP) and FDA guidelines mimic the GI tract envi...

Hydrotropy is one of the solubilizing techniques to enhance the solubility of poorly water solubl... more Hydrotropy is one of the solubilizing techniques to enhance the solubility of poorly water soluble drugs. In the present investigation, hydrotropic solution of sodium citrate (0.1M) was employed as solubilizing agent to solubilize the poorly water soluble drug Naproxen fine powder and its tablet dosage form for spectrophotometric determination in UV region. Naproxen shows maximum absorbance at 330 nm and follows Beer's law in concentration range of 20-140 mcg/mL. Results of analysis were statistically validated for the linearity, precision, LOD, and LOQ. The proposed method is new, simple, accurate, reliable, more economic and can be successfully employed in routine to analyze Naproxen tablets. Either hydrotropic agent or commonly used tablet additives did not interference in analysis. The percentage recovery was within the range between 99 and 100.

International Journal of Pharmaceutical Sciences Review and Research

A first derivative spectrofluorimetric method has been developed and validated for simultaneous q... more A first derivative spectrofluorimetric method has been developed and validated for simultaneous quantification of Nebivolol hydrochloride (NEB) and Valsartan (VAL) in combined tablet dosage form without any prior separation of components from the sample. NEB was determined at emission wavelength of 294 nm (zero-crossing wavelength point of VAL). Similarly, VAL was measured at 404 nm (zero-crossing wavelength point of NEB). The first derivative amplitude-concentration plots were rectilinear over the range of 0.1-2.1 µg/ml; for both drugs. Analytical performance of the proposed spectrofluorimetric procedure was statistically validated with respect to linearity, range, precision, accuracy, selectivity, detection and quantification limits as per ICH guidelines. No interference was observed from common pharmaceutical additives. The % assay in commercial formulation was found to be 101.6 and 98.5 for NEB and VAL, respectively by the proposed method and % RSD values for precision and accur...

Aim: Current work entails the analytical quality by design (AQbD) based robust HPLC method for re... more Aim: Current work entails the analytical quality by design (AQbD) based robust HPLC method for real-time analysis of canagliflozin and metformin. Different pKa values of two drugs made their chromatographic separation critical. Materials and Methods: The critical method parameters were systematically optimized using factorial experimental design (central composite design) and contours were generated as a function of significant variables when analyzed in the modeling software. The method operable design region that control the variation in response is obtained from contour plot and verified experimentally. Results: Effective chromatographic separation of title analytes was accomplished on SPOLAR C 18 (250 x 4.6 mm, 5µ) column at 25°C with mobile phase comprising of phosphate buffer, pH 6.0 and acetonitrile (55:45 % v/v), pumped at a flow rate of 0.8 mL/ min by isocratic elution pattern and UV detection at 254 nm. The linear model was established in the range of 50-300 and 5-30 and µg/mL at retention times of 3.24 and 10.77 min for metformin and canagliflozin, respectively. Conclusion: Method obeyed all validation parameters of ICH Q2 (R1) guidelines and able to discriminate the Adduct generated upon drug degradation. The proposed method was pertinent for assay drugs and extended to quantify the drugs in prevalence of biological matrix.

Journal of chromatographic science, 2021

New analytical quality by design-oriented HPLC method with multiple response optimization (Derrin... more New analytical quality by design-oriented HPLC method with multiple response optimization (Derringer's desirability function) was demonstrated for simultaneous analysis of three antidiabetic drugs (metformin hydrochloride/empagliflozin/linagliptin) in a fixed-dose combination. Central composite design was employed for systematic optimization of critical method parameters, namely, % organic phase (X1), aqueous phase pH (X2) and flow rate (X3) while resolution, capacity factor and theoretical plate number as critical analytical attributes. Effective chromatographic separation of title analytes was accomplished on Std. Discovery C18 column at 30°C with mobile phase comprising acetonitrile: phosphate buffer pH 5 (38:62% v/v), pumped at a flow rate of 1 mL/min by isocratic elution pattern and UV detection at 222 nm. The model is rectilinear in the range of 1.0-200, 0.2-40 and 0.1-20 μg/mL at retention times of 3.04, 3.93 and 5.99 min for metformin, empagliflozin and linagliptin, resp...

Future Journal of Pharmaceutical Sciences, 2021

Analytical quality by design driven HPLC method has been optimized for simultaneous estimation of... more Analytical quality by design driven HPLC method has been optimized for simultaneous estimation of dapagliflozin and saxagliptin in pharmaceutical dosage form. Response surface methodology was employed for optimization of experimental conditions using three factors such as organic phase (%), pH of aqueous phase, and flow rate of mobile phase. Virtuous separation of analytes was achieved with mobile phase consisted of acetonitrile: phosphate buffer, pH 5.8 (26:74% v/v) with flow rate 0.96 mL/min using SPOLAR C18 column (250 × 4.6 mm, 5 μ) with run time 6 min and UV detection at 236 nm. Retention time for dapagliflozin and saxagliptin were found to be 3.5 and 5.0 min, respectively. Method was validated as per ICH guidelines. The plot between peak area vs concentration for dapagliflozin and saxagliptin were rectilinear in the range of 0.2-300 μg/mL and 0.1-150 μg/mL respectively with detection and quantification limits were 0.061 and 0.18 μg/mL for dapagliflozin and 0.014 and 0.043 μg/m...

The Turkish Journal of Pharmaceutical Sciences

Amaç: Bu çalışmanın amacı tamsulosin hidroklorür ve solifenasin süksinatın aynı anda miktar tayin... more Amaç: Bu çalışmanın amacı tamsulosin hidroklorür ve solifenasin süksinatın aynı anda miktar tayininin yapılabilmesi için basit bir senkronize spektroflorimetri yöntemi geliştirmek ve valide etmektir. Gereç ve Yöntemler: Bahsedilen analitlerin aynı anda miktar tayinlerinin yapılabilmesi için birinci türev senkronize spektroflorimetri yöntemi kullanılmıştır. Tamsulosin hidroklorür 322 nm de ölçüm yapılarak (bu dalga boyu solifenasin süksinatın sıfır kesim noktasıdır) solifenasin süksinat ise 570 nm de ölçüm yapılarak (bu dalga boyu tamsulosin hidroklorürün sıfır kesim noktasıdır) miktar tayinleri gerçekleştirilmiştir. Bulgular: Kalibrasyon eğrileri tamsulosin hidroklorür için 2-10 μg/mL, solifenasin süksinat için ise 30-150 μg/mL konsantrasyon aralığında hazırlanmıştır. Geliştirilen yöntemle; ICH kılavuzlarına göre hesaplanan doğrusallık, seçicilik, doğruluk, kesinlik ve LOD ve LOQ değerleri kullanılarak başarılı sonuçlar elde edilmiştir. Önerilen yöntemle yapılan analiz sonuçları ticari formülasyon içerisinde tamsulosin hidroklorürün %95.0 solifenasin süksinatın ise %103.5 oranında bulunduğunu göstermiştir. Bu sonuçlar preparatın üzerinde belirtilen değerler ile iyi bir uygunluk göstermektedir. Sonuç: Önerilen analitik yöntemin tablet dozaj formlarında tamsulosin hidroklorür ve solifenasin süksinatın rutin kontrol analizlerinde kullanılabileceği anlaşılmıştır. Anahtar kelimeler: Tamsulosin hidroklorür, solifenasin süksinat, senkronize spektroflorimetri, yöntem validasyonu Objectives: The present study was undertaken with the objective to develop and validate a simple spectrofluorimetric method for the simultaneous quantification of tamsulosin hydrochloride and solifenacin succinate. Materials and Methods: First-derivative synchronous spectrofluorimetry was attempted for the simultaneous quantification of the analytes. Tamsulosin hydrochloride was quantified at a wavelength of 322 nm (zero-crossing wavelength point of solifenacin succinate) and solifenacin succinate was measured at 570 nm (zero-crossing wavelength point of tamsulosin hydrochloride). Results: Calibration plots were constructed over the concentration range of 2-10 μg/mL for tamsulosin hydrochloride and 30-150 μg/mL for solifenacin succinate. The method gave satisfactory results when it is validated for linearity, specificity, accuracy, precision, LOD and LOQ as per the ICH guidelines. The assay values in the commercial formulation were found to be in the percentage range of 95.0 for tamsulosin hydrochloride and 103.5 for solifenacin succinate by the proposed method. These results were well in agreement with their label claim. Conclusion: The proposed synchronous analytical method can be employed for routine quality control analysis of tamsulosin hydrochloride/ solifenacin succinate in tablet dose forms.

INDIAN DRUGS

A simple and sensitive spectrofluorimetric method has been developed for the estimation of mesala... more A simple and sensitive spectrofluorimetric method has been developed for the estimation of mesalamine (MES). Linearity was obeyed in the range of 0.1-2.5 µg/mL in distilled water as solvent at an emission wavelength (λem) of 501 nm after excitation (λex) at 332 nm, with a good correlation coefficient of 0.999. The limit of detection and limit of quantification for this method were 0.05 and 0.1 µg/mL, respectively. The developed method was statistically validated as per ICH guidelines. The percentage relative standard deviation values were found to be less than 2 for accuracy and precision studies. The assay results obtained were in good agreement with the labeled amounts of the marketed formulations. This validated method was extended to study the degradation behavior of mesalamine in various conditions such as acid, alkaline, oxidative, thermal, and UV effects. Although there was no degradation observed in oxidative, thermal, UV effect, 41.9 % and 11.6 % amount was degraded in acid...

Turkish Journal of Pharmaceutical Sciences

Future Journal of Pharmaceutical Sciences

Background A simple and sensitive spectrophotometric method was developed for the quantitative me... more Background A simple and sensitive spectrophotometric method was developed for the quantitative measurement of dolutegravir in pure form and pharmaceutical formulation. The present method was based on redox reaction between dolutegravir and ferric chloride, which upon complexation with 1,10-phenanthroline formed an orange-colored complex that showed absorption maximum at 520.0 nm. Results The developed method obeyed linearity in the concentration range of 40.00–140.00 μg/mL. The method was also validated as per International Council for Harmonization guidelines and the results were within acceptance values. The validated method was employed for the determination of dolutegravir in pharmaceutical dosage form and the percentage assay value was found to be 102.5, which is in agreement with its label claimed. Conclusion The developed redox-based colorimetric method could be used in the routine quality control analysis of dolutegravir present in various pharmaceutical dosage forms.

Journal of Applied Pharmacy

Purpose: In this present work a simple, rapid, specific and highly sensitive spectrofluorimetric ... more Purpose: In this present work a simple, rapid, specific and highly sensitive spectrofluorimetric method was developed and validated for the quantification of tapentadol HCl bulk drug and pharmaceutical dosage forms and proposed method was also applied to study of forced degradation and in-vitro dissolution studies. Materials and Methods: The fluorescence intensity of tapentadol HCl in distilled water was measured at emission wavelength 592 nm after excitation at 272 nm by using a Shimadzu (Japan) RF-5301 PC spectrofluorophotometer. A linear relationship was found between fluorescence intensity and concentration in the range of 1-6 µg/mL with a good correlation coefficient-0.999. Results: The detection and quantification limits were found to be 23.01 and 76.72 ng/mL, respectively. The proposed method was applied for quantification of tapentadol HCl in tablets, with percentage recovery of 99.95-101.45% and percentage RSD values were found to be less than 2 for accuracy and precision studies. Statistical analysis of the results revealed high accuracy and good precision. Conclusion: The suggested procedures could be used for the determination of tapentadol HCl in drug substance and drug products as well as in presence of its degradation products.

Journal of Applied Pharmacy

A reverse phase stability indicating HPLC method was developed for the analysis of efavirenz bulk... more A reverse phase stability indicating HPLC method was developed for the analysis of efavirenz bulk and pharmaceutical formulations. The developed method was also utilized for in-vitro dissolution studies of efavirenz formulations. Acetonitrile and acetate buffer pH 3.4 was the mobile phase (75:25% v/v), with retention time of 4.007 min at a flow rate of 1.5 mL/min detected at 292 nm wavelength. Linear regression analysis calibration plot showed an excellent linearity between response and concentration in the range of 50-300 μgmL-1. The regression coefficient was 0.999 and the linear regression equation was y = 7780x+11159. Limits of detection (LOD) and quantification (LOQ) were 0.238 and 0.793 μgmL-1 respectively. The method was validated for accuracy, precision, specificity, robustness, detection and quantification limits, in accordance with ICH guidelines. The specificity of the method was ascertained by forced degradation studies by acid, alkali hydrolysis, oxidation and thermal degradation methods. The degraded products were well resolved from the analysis peak with significant differences at their retention time values. Wide linearity range, sensitivity, accuracy, short retention time and simple mobile phase indicate the method is suitable for routine quantification of efavirenz with high precision and accuracy.

Indian Journal of Pharmaceutical Education and Research

Aim: Current work entails the analytical quality by design (AQbD) based robust HPLC method for re... more Aim: Current work entails the analytical quality by design (AQbD) based robust HPLC method for real-time analysis of canagliflozin and metformin. Different pKa values of two drugs made their chromatographic separation critical. Materials and Methods: The critical method parameters were systematically optimized using factorial experimental design (central composite design) and contours were generated as a function of significant variables when analyzed in the modeling software. The method operable design region that control the variation in response is obtained from contour plot and verified experimentally. Results: Effective chromatographic separation of title analytes was accomplished on SPOLAR C 18 (250 x 4.6 mm, 5µ) column at 25°C with mobile phase comprising of phosphate buffer, pH 6.0 and acetonitrile (55:45 % v/v), pumped at a flow rate of 0.8 mL/ min by isocratic elution pattern and UV detection at 254 nm. The linear model was established in the range of 50-300 and 5-30 and µg/mL at retention times of 3.24 and 10.77 min for metformin and canagliflozin, respectively. Conclusion: Method obeyed all validation parameters of ICH Q2 (R1) guidelines and able to discriminate the Adduct generated upon drug degradation. The proposed method was pertinent for assay drugs and extended to quantify the drugs in prevalence of biological matrix.

Turkish Journal of Pharmaceutical Sciences

Prazikuantel miktar tayini için basit, hızlı, spesifik ve yüksek duyarlılığa sahip, çevre dostu s... more Prazikuantel miktar tayini için basit, hızlı, spesifik ve yüksek duyarlılığa sahip, çevre dostu spektrofluorimetrik bir yöntem geliştirilmiştir. Gereç ve Yöntemler: Prazikuantel konsantrasyonu ile floresan yoğunluğu arasında, 1-20 μg/mL aralığında su içinde, 286 nm emisyon ve 263 nm eksitasyon dalga boyunda, iyi bir korelasyon katsayısı (0.999) olan doğrusal bir ilişki bulundu. Bulgular: Önerilen yöntem Uluslararası Uyumlaştırma Konferansı yönergelerine göre doğrulanmıştır ve sonuçların istatistiksel analizi, 2'den düşük bağıl standart sapma değerleri ile yüksek doğruluk ve hassasiyet göstermiştir. Saptama ve miktar limitleri sırasıyla 0.27 ve 0.81 μg/mL'dir. Önerilen yöntem, ilacın stabilitesini ve asidik, alkali ve oksidatif koşullar varlığında bozunma kinetiklerini araştırmak için genişletilmiştir. Sonuç: Yöntem, prazikuantel tablet formülasyonunun in vitro çözünme çalışmaları için kullanılmıştır. Önerilen prosedürler, prazikuantelin ilaç maddesi ve ilaç ürünlerinde ve degradasyon ürünlerinin varlığının değerlendirilmesi için kullanılabilir. Anahtar kelimeler: Prazikuantel, eksitasyon dalga boyu-263 nm, emisyon dalga boyu-286 nm, çözünme, zorla bozunma Objectives: A simple, rapid, specific, and highly sensitive ecofriendly spectrofluorimetric method has been developed for the quantification of praziquantel. Materials and Methods: A linear relationship was found between fluorescence intensity and praziquantel concentration in the range of 1-20 μg/mL in water at emission wavelength of 286 nm after excitation wavelength at 263 nm with a good correlation coefficient (0.999). Results: The proposed method was validated according to International Conference on Harmonization guidelines and statistical analysis of the results revealed high accuracy and good precision with the percentage relative standard deviation values less than 2. The detection and quantification limits were 0.27 and 0.81 μg/mL, respectively. The proposed method was extended to investigate the stability of the drug and its degradation kinetics in the presence of acidic, alkaline, and oxidative conditions. Conclusion: The method was utilized for in vitro dissolution studies of praziquantel tablet formulation. The suggested procedures could be used for the assessment of praziquantel in drug substance and drug products as well as in the presence of its degradation products.

Turkish Journal of Pharmaceutical Sciences

Amaç: Günümüzde, çeşitli dozaj formlarında etkin madde kombinasyonlarına rağbet edilmektedir, anc... more Amaç: Günümüzde, çeşitli dozaj formlarında etkin madde kombinasyonlarına rağbet edilmektedir, ancak bunlardaki etkin maddeleri tayin etmek için farmakope yöntemleri bulunmamaktadır. Bu çalışmada, kombine dozaj formunun analizi için kalite kontrol testini sadeleştirmek amacıyla tek bir çözünme testi yöntemi tercih edilmiştir. Gereç ve Yöntemler: Suda çözünürlüğü sınırlı olan ilacın çözünme yöntemi için geliştirilen çözünme ortamı in vivo davranışlarının kalitatif tahmininde biyouyumlu bir yöntem olarak kullanışlı bulunmuştur. Bulgular: Atorvastatin ve fenofibrat içeren kapsüllerde çözünme profilleri, 37±0.5°C'de, 50 rpm ve 900 mL ortam içinde bir palet tipi Amerikan Farmakopesi çözünme cihazı ile değerlendirildi. En iyi ortam, 900 mL %0.5 a/h sodyum lauril sülfattır. Piyasadaki tabletler için kümülatif % çözünme, 45 dakika içinde %85'ten fazla olmuştur. Önerilen çözünme testi koşulları ayırt edici bir güce sahiptir, farklılık faktörü (f 1) değerleri düşüktür (%12-16) ve benzerlik (f 2) faktör değerleri de düşüktür (%45-48). Bu nedenle, %0.5 w/v sodyum lauril sülfat çözeltisinin kullanımı uygundur. Objectives: Nowadays, the market is flooded with combinations of drugs in various dosage forms, but there is a lack of official methods to quantify them. A single dissolution test method for the analysis of combined dosage form is preferred for simplification of quality control testing. Materials and Methods: If the developed dissolution medium mimics the biorelevant and discriminating dissolution procedure for drug products with limited drug aqueous solubility it is a useful tool for qualitative forecasting of the in vivo behavior of formulations. Results: Dissolution profiles were evaluated for atorvastatin and fenofibrate in capsules, using a paddle-type United States Pharmacopeia dissolution apparatus in 900 mL of medium at 50 rpm and 37±0.5°C. The best medium was 900 mL of 0.5% w/v sodium lauryl sulfate. The cumulative % dissolution was more than 85% within 45 min for marketed tablets. The proposed dissolution test conditions have discriminative power, dissimilarity factor (f 1) values are low (12-16%), and similarity (f 2) factor values are also low (45-48%). Hence the use of 0.5% w/v sodium lauryl sulfate solution is justified. Conclusion: The dissolution method was validated (% relative standard deviation <2). To quantify both drugs simultaneously, a second derivative spectrophotometric method was established (λ max 281 nm and 296 nm, respectively, for atorvastatin and fenofibrate) in acetate buffer, pH 2.8 solution.

Turkish Journal of Pharmaceutical Sciences

spectrophotometric methods have been developed and validated for quantification of Lornoxicam (LO... more spectrophotometric methods have been developed and validated for quantification of Lornoxicam (LOR) and Mesalamine (MES) drugs in pure form and in pharmaceutical formulations. MATERIALS AND METHODS: Shimadzu Double-beam UV-Visible Spectrophotometer 1800 having spectral bandwidth of 0.1 nm with wavelength accuracy ±0.1 nm and a pair of 1 cm path length matched quartz cells were used to measure absorbance of the resulting solution. Method (I) is used for the quantification of LOR which is based on the measurement of absorbance of bluish green coloured chromogen complex at 760 nm which is formed by reaction of LOR with ferric chloride and potassium ferricyanide (redox technique). Method (II) is used for the quantification of MES that is based on measurement of absorbance of yellow coloured chromogen at 400 nm which is formed by the condensation reaction of the primary amino group of MES with salicylaldehyde reagent (SA) (Schiff base formation). RESULTS: Both the methods obeyed Beer's law in concentration range of 0.5-4.5 μg/mLand 0.2-1.7 μg/mL with good correlation coefficients of 0.9974 and 0.998 for Methods (I) and (II) respectively. CONCLUSION: The developed method is simple, sensitive, specific which is validated statistically as per ICH guidelines and can be used in routine analysis of LOR and MES pharmaceutical dosage forms.

International Journal of Research in Pharmaceutical and Biomedical Sciences

____________________________________________________________________________________ A simple, ra... more ____________________________________________________________________________________ A simple, rapid accurate and stability indicating RP-HPLC method was developed for the determination of Capecitabine in pure and tablet dosage form. The method showed a linear response for concentrations in the range of 70-120 µg/ml using 0.05M phosphate buffer (p H 3.0 ± 0.05) buffer and acetonitrile (50:50 % w/v) as the mobile phase with detection at 240 nm and a flow rate of 1 mL/min and retention time 4.108 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, forced degradation, solution stability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from recovery studies was found to be less than 1. The specificity of the method was ascertained by forced degradation studies by acid, alkali hydrolysis, oxidation and thermal degradation. The degraded products were well resolved from th...

Asian Journal of Pharmaceutical and Clinical Research

Dissolution process is considered as an important in vitro tool for evaluating the bioequivalence... more Dissolution process is considered as an important in vitro tool for evaluating the bioequivalence of products. Such a method, if properly mimic the in vivo conditions, it would surrogate the in vivo studies. Bioequivalence problems arise in class-II and class-IV categories of Biopharmaceutical Classification of Drugs (BCS). Efavirenz (BCS Class II drug) is used in active anti retroviral therapy. Saturation solubility of efavirenz bulk drug was evaluated in various surfactant media, pH solutions and bio-relevant media. We optimized the dissolution conditions for efavirenz with 900 ml of simulated gastric fluid with 0.25% w/v sodium lauryl sulphate (SGF-0.25% w/v SLS) as discriminating and bio-relevant dissolution medium at 50 rpm for 45 min (5 min time interval) with USP apparatus II. The optimized media contained a less amount of SLS (0.25% w/v) in SGF compared with 1% and 2% SLS concentration stated in the official monographs (IP, BP, USP) and FDA guidelines mimic the GI tract envi...

Hydrotropy is one of the solubilizing techniques to enhance the solubility of poorly water solubl... more Hydrotropy is one of the solubilizing techniques to enhance the solubility of poorly water soluble drugs. In the present investigation, hydrotropic solution of sodium citrate (0.1M) was employed as solubilizing agent to solubilize the poorly water soluble drug Naproxen fine powder and its tablet dosage form for spectrophotometric determination in UV region. Naproxen shows maximum absorbance at 330 nm and follows Beer's law in concentration range of 20-140 mcg/mL. Results of analysis were statistically validated for the linearity, precision, LOD, and LOQ. The proposed method is new, simple, accurate, reliable, more economic and can be successfully employed in routine to analyze Naproxen tablets. Either hydrotropic agent or commonly used tablet additives did not interference in analysis. The percentage recovery was within the range between 99 and 100.

International Journal of Pharmaceutical Sciences Review and Research

A first derivative spectrofluorimetric method has been developed and validated for simultaneous q... more A first derivative spectrofluorimetric method has been developed and validated for simultaneous quantification of Nebivolol hydrochloride (NEB) and Valsartan (VAL) in combined tablet dosage form without any prior separation of components from the sample. NEB was determined at emission wavelength of 294 nm (zero-crossing wavelength point of VAL). Similarly, VAL was measured at 404 nm (zero-crossing wavelength point of NEB). The first derivative amplitude-concentration plots were rectilinear over the range of 0.1-2.1 µg/ml; for both drugs. Analytical performance of the proposed spectrofluorimetric procedure was statistically validated with respect to linearity, range, precision, accuracy, selectivity, detection and quantification limits as per ICH guidelines. No interference was observed from common pharmaceutical additives. The % assay in commercial formulation was found to be 101.6 and 98.5 for NEB and VAL, respectively by the proposed method and % RSD values for precision and accur...

Aim: Current work entails the analytical quality by design (AQbD) based robust HPLC method for re... more Aim: Current work entails the analytical quality by design (AQbD) based robust HPLC method for real-time analysis of canagliflozin and metformin. Different pKa values of two drugs made their chromatographic separation critical. Materials and Methods: The critical method parameters were systematically optimized using factorial experimental design (central composite design) and contours were generated as a function of significant variables when analyzed in the modeling software. The method operable design region that control the variation in response is obtained from contour plot and verified experimentally. Results: Effective chromatographic separation of title analytes was accomplished on SPOLAR C 18 (250 x 4.6 mm, 5µ) column at 25°C with mobile phase comprising of phosphate buffer, pH 6.0 and acetonitrile (55:45 % v/v), pumped at a flow rate of 0.8 mL/ min by isocratic elution pattern and UV detection at 254 nm. The linear model was established in the range of 50-300 and 5-30 and µg/mL at retention times of 3.24 and 10.77 min for metformin and canagliflozin, respectively. Conclusion: Method obeyed all validation parameters of ICH Q2 (R1) guidelines and able to discriminate the Adduct generated upon drug degradation. The proposed method was pertinent for assay drugs and extended to quantify the drugs in prevalence of biological matrix.