scholarly journals High-Performance Liquid Chromatographic and First Derivative of the Ratio Spectrophotometric Determination of Amlodipine and Valsartan in Their Binary Mixtures

2010 ◽  
Vol 93 (3) ◽  
pp. 882-890 ◽  
Author(s):  
Dilek Kul ◽  
Burcu Dogan-Topal ◽  
Tugba Kutucu ◽  
Bengi Uslu ◽  
Sibel A Ozkan
Keyword(s):  
Spectrophotometric Method ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Time Saving ◽  
Pharmaceutical Dosage Form ◽  
First Derivative ◽  
Significant Difference ◽  
Long Acting

Abstract Amlodipine besylate (AML) is a long-acting calcium channel blocker used as an antihypertensive agent. Valsartan (VAL) is also used to treat hypertension, either alone or in combination with other agents. Two-component mixtures of AML and VAL were analyzed by HPLC and the ratio spectra of the first derivative spectrophotometric technique. The spectrophotometric method depends on the first derivative of the ratio-spectra by measurements of the amplitudes at 234.0 nm for VAL and 351.0 nm for AML. Calibration graphs were established for 0.520 g/mL AML and 132 g/mL VAL using the ratio spectra of the first derivative spectrophotometric method. In the HPLC method, an ACE 5 C18 (4.6 150 mm, 5 m) RP column at 30C with the mobile phase methanolacetonitrileNaH2PO4H2O buffer, including 5 mL/L triethylamine and adjusted to pH 3.0 (42 + 18 + 40, v/v/v) at 2.0 mL/min flow rate was used to separate both compounds with detection at 254.0 nm. Linearity was obtained in the concentration range of 0.5500 g/mL for AML and 5.0900 g/mL for VAL. The proposed methods have been extensively validated. These methods allow a number of cost- and time-saving benefits. They were successfully applied to the determination of AML and VAL in synthetic mixtures and in a pharmaceutical dosage form. There was no significant difference between the performance of the proposed methods regarding the mean and SD values. The proposed methods are simple, rapid, and suitable for QC applications.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF ATOMOXETINE HYDROCHLORIDE USING RAPID HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC TECHNIQUE

2018 ◽  
Vol 11 (11) ◽  
pp. 118
Author(s):  
Zubaidur Rahman ◽  
Vijey Aanandhi M ◽  
Sumithra M
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Sensitivity ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Chromatographic Technique ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Liquid Chromatographic

Objective: A simple, novel, sensitive, rapid high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for quantitative determination of atomoxetine HCl (ATH) in bulk and formulations.Methods: The chromatographic development was carried out on RP-HPLC. The column used as Xterra RP 18 (250 mm × 4.6 mm, 5 μ particle size), with mobile phase consisting of methanol: water 80:20 V/V. The flow rate was 1.0 mL/min and the effluents were monitored at 270 nm.Results: The retention time was found to be 5.350 min. The method was validated as per International Conference on Harmonization Guideline with respect to linearity, accuracy, precision, and robustness. The calibration curve was found to be linear over a range of 2–10 μg/mL with a regression coefficient of 0.9999. The method has proved high sensitivity and specificity.Conclusion: The results of the study showed that the proposed RP-HPLC method was simple, rapid, precise and accurate which is useful for the routine determination of ATH in bulk drug and in its pharmaceutical dosage form.

scholarly journals A Comparative Study of First-Derivative Spectrophotometry and Column High-Performance Liquid Chromatography Applied to the Determination of Repaglinide in Tablets and for Dissolution Testing

2008 ◽  
Vol 91 (3) ◽  
pp. 530-535 ◽  
Author(s):  
Bashar A AlKhalidi ◽  
Majed Shtaiwi ◽  
Hatim S AlKhatib ◽  
Mohammad Mohammad ◽  
Yasser Bustanji
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Spectroscopic Method ◽  
High Performance Liquid Chromatographic ◽  
Dissolution Testing ◽  
First Derivative ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Significant Difference

Abstract A fast and reliable method for the determination of repaglinide is highly desirable to support formulation screening and quality control. A first-derivative UV spectroscopic method was developed for the determination of repaglinide in tablet dosage form and for dissolution testing. First-derivative UV absorbance was measured at 253 nm. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ) in comparison to the U.S. Pharmacopeia (USP) column high-performance liquid chromatographic (HPLC) method. The first-derivative UV spectrophotometric method showed excellent linearity [correlation coefficient (r) = 0.9999] in the concentration range of 135 g/mL and precision (relative standard deviation <1.5). The LOD and LOQ were 0.23 and 0.72 g/mL, respectively, and good recoveries were achieved (98101.8). Statistical comparison of results of the first-derivative UV spectrophotometric and the USP HPLC methods using the t-test showed that there was no significant difference between the 2 methods. Additionally, the method was successfully used for the dissolution test of repaglinide and was found to be reliable, simple, fast, and inexpensive.

scholarly journals Development and validation of stability indicating RP-HPLC method for the determination of Epinastine Hydrochloride in Pharmaceutical dosage form

1970 ◽  
Vol 1 (3) ◽  
pp. 50-55 ◽  
Author(s):  
Aparajita Malakar ◽  
Bishwajit Bokshi
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Dosage Form ◽  
Active Pharmaceutical Ingredient ◽  
Pharmaceutical Journal ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

A simple, specific, accurate and stability-indicating high performance liquid chromatographic method was developed and validated for the determination of Epinastine Hydrochloride in pharmaceutical dosage form. The chromatographic conditions comprised of a reverse-phase, C18 column (150×4.6 mm), 5μm with a mobile phase consisting of a mixture of aqueous phase (3.8g of sodium pantanesulphonate monohydrate and 4.0g of potassium dihydrogen orthophosphate was dissolved in 1L of water and pH of solution was adjusted to 4.5 with o-phosphoric acid) and organic phase (acetonitrile and methanol was mixed in the ratio of 4:1 v/v) in the ratio of 60:40 v/v at a flow rate of 1.0ml/min. Detection was carried out at 220nm. The retention time of Epinastine Hydrochloride was found to be 3.5 min. The calibration curve was found linear between 2-200μg/ml. The percentage recoveries of Epinastine Hydrochloride were found to be in the range of 99.05-100.50%. The method was validated for accuracy, linearity, precision, detection limit, quantitation limit and robustness. The drug was subjected to acidic hydrolysis, basic hydrolysis, neutral hydrolysis, oxidation, photochemical and thermal degradation. All the peaks of degraded product were resolved from the active pharmaceutical ingredient with significantly different retention time. As the method could effectively separate the drug from its degradation product, it can be employed as a stability indicating one. Key Words: Epinastine hydrochloride; validation; stability indicating method; HPLC; dosage form. DOI: http://dx.doi.org/10.3329/icpj.v1i3.9662 International Current Pharmaceutical Journal 2012, 1(3): 50-55

scholarly journals Development and Validation of Column High-Performance Liquid Chromatographic and Derivative Spectrophotometric Methods for Determination of Levofloxacin and Ornidazole in Combined Dosage Forms

2008 ◽  
Vol 91 (4) ◽  
pp. 756-761 ◽  
Author(s):  
Satish A Patel ◽  
Arun M Prajapati ◽  
Paresh U Patel ◽  
Natubhai J Patel ◽  
Jayesh B Vaghmasi
Keyword(s):  
Spectrophotometric Method ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Zero Crossing ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Rp Hplc ◽  
Liquid Chromatographic

Abstract The manuscript describes validated reversed-phase column high-performance liquid chromatographic (RP-HPLC) and first-derivative UV spectrophotometric methods for the estimation of levofloxacin (LFX) and ornidazole (ORNI) in combined dosage forms. The RP-HPLC separation was achieved on a Phenomenex C18 column (250 mm 4.6 mm id, 5 m) using KH2PO4 buffer (pH 6.8)methanolacetonitrile (70 + 15 + 15, v/v/v) mobile phase at a flow rate of 1.5 mL/min and ambient temperature (25 2<sup/>C). Quantification was achieved with photodiode array detection at 295 nm over the concentration range of 110 g/mL for both LFX and ORNI, with mean recovery of 101.7 0.23 and 99.23 1.57, respectively, by the RP-HPLC method. The derivative spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first-order derivative spectra were obtained at N =1 (scaling factor), = 2.0 nm (wavelength interval), and the determinations were made at 310 nm (ZCP of ORNI) for LFX and 295 nm (ZCP of LFX) for ORNI over the concentration range of 240 g/mL for both LFX and ORNI. Mean recovery was 99.46 0.96 and 100.9 0.72, respectively, by the first-derivative UV spectrophotometric method. Standard and sample solutions were prepared with methanol as the solvent in both of the methods. These methods were found to be simple, accurate, precise, and sensitive and were applicable for the simultaneous determination of LFX and ORNI in combined dosage forms.

scholarly journals Development of Stability Indicating LC Method for the Estimation of Tolperisone in Bulk and Pharmaceutical Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
U. K. Chhalotiya ◽  
K. K. Bhatt ◽  
D. A. Shah ◽  
S. L. Baldania ◽  
S. B. Patel
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Chemical Oxidation ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Significant Difference ◽  
Alkali Hydrolysis

A rapid, specific, and sensitive reverse phase high performance liquid chromatographic method has been developed and validated for analysis of tolperisone in both bulk and pharmaceutical dosage form. The HPLC method was performed with a reversed phase C18 SunFire column (250 mm × 4.6 mm i.d., 5 mm particle size), detection at 261 nm and a mixture of methanol, water and pH 7.5 adjusted by use of 1% solution of triethylamine (60 : 40) as mobile phase. The flow rate was 1.0 mL min−1 and effluents were monitored at 261 nm. The retention time of tolperisone was 4.8 min. Tolperisone was subjected to acid and alkali hydrolysis, chemical oxidation, wet hydrolysis, dry heat degradation, and sunlight degradation. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time values. Stressed samples were assayed using developed LC method. The proposed method was validated with respect to linearity, accuracy, precision, and robustness. The method was successfully applied to the estimation of tolperisone in tablet dosage forms.

scholarly journals RP-HPLC Method Development and Validation for Determination of Tigecycline in Bulk and Pharmaceutical Dosage form

2021 ◽  
pp. 273-282
Author(s):  
K. Bhavyasri ◽  
C. H. Mounika ◽  
Narmada Vallakeerthi ◽  
M. Sumakanth
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Good Precision ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Water Ph

Aims: To develop and validate a new, simple, rapid, precise and accurate Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method for the quantitative determination of Tigecycline in bulk and pharmaceutical dosage form. Study Design: Place and Duration of the Study: RBVRR women's college of pharmacy, Barkatpura, Hyderabad, between june 2019 and july 2020. Methodology: The RP-HPLC method was developed on Sunsil C18 150 mm x 4.6mm x 5µ column using acetonitrile : water (pH maintained at 3.5 with acetic acid) [70:30] as mobile phase at flow rate 0.8 ml/min and UV detection at 250 nm. Results: Tigecycline exhibited linearity over the concentration range of 5-40 µg/mL (R2 > 0.999). The analytical method showed good precision with % RSD below 2. The method showed suitable accuracy and robustness. Conclusion: Validation of the developed method was done as per International Conference on Harmonization (ICH) Q2R1 guidelines.

HPLC method for the determination of the S- and R-diastereomers of telaprevir for treatment of patients with hepatitis C

2015 ◽  
Vol 39 (3) ◽  
Author(s):  
Werner J. Heinz ◽  
Dieter Kuschak ◽  
Diana Schirmer ◽  
Anna Grau ◽  
Daniela Keller ◽  
...  
Keyword(s):  
Hepatitis C ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Clinical Samples ◽  
Coefficients Of Variation ◽  
Significant Difference ◽  
High Degree ◽  
Liquid Chromatographic

AbstractTelaprevir (TVR) was approved by the FDA in May 2011 for the treatment of hepatitis C. This protease inhibitor converts into two diastereomers with significant difference in antiviral activity. Clinical efficacy has been correlated with serum concentrations. Therefore, a sensitive and selective high-performance liquid chromatographic method for the simultaneous determination of both clinically relevant diastereomers of TVR was developed. Linearity ranged from 20 to 10,000 ng/mL. The coefficients of variation were <7.3%, and accuracy was between −4.0 and 5.4%. In 105 clinical samples, both diastereomers of TVR had a high degree of correlation to each other, but concentrations showed a broad range and an increase during therapy.

VALIDATED RP-HPLC METHOD FOR DETERMINATION OF ENZALUTAMIDE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (11) ◽  
pp. 46-50
Author(s):  
Z. G Khan ◽  
◽  
S. S. Patil ◽  
P. K. Deshmukh ◽  
P. O. Patil
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detector ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Bulk Drug

Novel, isocratic reversed phase high performance liquid chromatography method was developed and validated for the determination of enzalutamide (EZA) in bulk drug and pharmaceutical formulation. Efficient separation was achieved on PrincetonSPHER C18 100A, 5μ (250×4.6 mm) under the isocratic mode of elution using acetonitrile: water (80:20) % V/V as a mobile phase pumped in to the column at flow rate 1.0 mL/min. The effluent was monitored at 237.0 nm using UV detector. EZA was eluted in the given mobile phase at retention time (tR) of 3.2 minutes. The standard calibration curve was linear over the concentration range 10 - 60 μg/mL with correlation coefficient 0.997. The method was validated for accuracy, precision, sensitivity, robustness, ruggedness and all the resulting data treated statistically. The system suitability parameters like retention time, theoretical plates, tailing factor, capacity factor were found within the limit.

scholarly journals Determination of Dyclonine Hydrochloride by a HPLC Method and Camphor and Menthol by a GC Method in Compound Lotion

2013 ◽  
Vol 2013 ◽  
pp. 1-4
Author(s):  
Suying Ma ◽  
Haixia Lv ◽  
Xiaojun Shang
Keyword(s):  
Retention Time ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Ionization Detector ◽  
Uv Detector ◽  
Flame Ionization ◽  
Liquid Chromatographic

A high performance liquid chromatographic (HPLC) method with UV detector for the determination of dyclonine hydrochloride and a gas chromatography (GC) method with flame ionization detector (FID) for the determination of camphor and menthol in lotion were developed. The developed HPLC method involved using a SinoChoom ODS-BP C18reversed-phase column (5 μm, 4.6 mm × 200 mm) and mobile phase consisting of acetonitrile : water : triethylamine in a ratio of 45 : 55 : 1.0; pH was adjusted to 3.5 with glacial acetic acid. The developed GC method for determination of camphor and menthol involved using an Agilent 19091J-413 capillary chromatographic column (30 m × 320 μm × 0.25 μm). The two methods were validated according to official compendia guidelines. The calibration of dyclonine hydrochloride for HPLC method was linear over the range of 20–200 μg/mL. The retention time was found at 6.0 min for dyclonine hydrochloride. The calibration of camphor and menthol of GC method was linear over the range of 10–2000 μg/mL. The retention time was found at 2.9 min for camphor and 3.05 min for menthol. The proposed HPLC and GC methods were proved to be suitable for the determination of dyclonine hydrochloride, camphor, and menthol in lotion.

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