scholarly journals Enantioseparation of Citalopram by RP-HPLC, Using Sulfobutyl Ether-β-Cyclodextrin as a Chiral Mobile Phase Additive

2016 ◽  
Vol 2016 ◽  
pp. 1-7 ◽  
Author(s):  
Yangfeng Peng ◽  
Quan Sophia He ◽  
Jiang Cai
Keyword(s):  
Mobile Phase ◽  
Ph Value ◽  
Limit Of Detection ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Aqueous Buffer ◽  
Rp Hplc ◽  
Chiral Mobile Phase Additive ◽  
Mobile Phase Additive ◽  
Limit Of Quantitation

Enantiomeric separation of citalopram (CIT) was developed using a reversed phase HPLC (RP-HPLC) with sulfobutylether-β-cyclodextrin (SBE-β-CD) as a chiral mobile phase additive. The effects of the pH value of aqueous buffer, concentration of chiral additive, composition of mobile phase, and column temperature on the enantioseparation of CIT were investigated on the Hedera ODS-2 C18column (250 mm × 4.6 mm × 5.0 um). A satisfactory resolution was achieved at 25°C using a mobile phase consisting of a mixture of aqueous buffer (pH of 2.5, 5 mM sodium dihydrogen phosphate, and 12 mM SBE-β-CD), methanol, and acetonitrile with a volumetric ratio of 21 : 3 : 1 and flow rate of 1.0 mL/min. This analytical method was evaluated by examining the precision (lower than 3.0%), linearity (regression coefficients close to 1), limit of detection (0.070 µg/mL for (R)-CIT and 0.076 µg/mL for (S)-CIT), and limit of quantitation (0.235 µg/mL for (R)-CIT and 0.254 µg/mL for (S)-CIT).

scholarly journals STABILITY-INDICATING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR DETERMINATION OF ANTIHISTAMINE DRUG AZELASTINE

2018 ◽  
Vol 11 (8) ◽  
pp. 248
Author(s):  
Shital Patel ◽  
Pasha Ty
Keyword(s):  
Nasal Spray ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Research Work ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: The objective of this research was to develop a simple, precise, accurate, and stability-indicating reverse-phase high-performance liquid chromatographic method for estimation of azelastine hydrochloride (AZL) in nasal spray preparation.Methods: Chromatography was performed on a 250 mm×4.6 mm, 5-μm particle size, Waters Spherisorb CN column using (50:50 v/v) mixture of potassium dihydrogen phosphate buffer and acetonitrile as mobile phase. The detection was carried out at 290 nm and flow rate employed was 1.0 ml/min. The degradation of AZL was studied under different ICH recommended stress conditions.Results: The retention time was 4.34 min for AZL. Linearity was established in the concentration range of 5–120 μg/ml, with a correlation coefficient of 0.9996. Limit of detection (LOD) and limit of quantitation (LOQ) were found to be 0.81 μg/ml and 2.44 μg/ml, respectively. Percentage recovery was found between 99 and 102%. The values of percentage relative standard deviation (<2%) proved the high precision of the proposed method. The method was found to be robust regarding any small variation in the column temperature, pH of mobile phase, and mobile phase ratio. AZL was found stable in 5 M HCl at 80°C for 5 h, 5 M NaOH at 80°C for 5 h, 30% H2O2 at 80°C for 5 h, and in oven at 70°C for 8 h.Conclusion: The results obtained in this research work clearly proved that the proposed HPLC method for the assay of AZL in nasal spray preparation is simple, precise, specific, accurate, and stability indicating. It indicates that the method is suitable for analysis of AZL in the raw material and the pharmaceutical product without interference from excipients.

scholarly journals A Fast and Validated HPLC Method for Simultaneous Determination of Dopamine, Dobutamine, Phentolamine, Furosemide, and Aminophylline in Infusion Samples and Injection Formulations

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Fuchao Chen ◽  
Baoxia Fang ◽  
Sicen Wang
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Stability Study ◽  
Precision Data ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Limit Of Quantitation ◽  
The Stability

A simple, fast, and validated HPLC method was developed for the simultaneous quantization of five cardiovascular agents: dopamine (DPM), dobutamine (DBM), phentolamine (PTM), furosemide (FSM), and aminophylline (APL) either in infusion samples or in an injection dosage form. The proposed method was achieved with a 150 mm × 4.6 mm, 5.0 μm C18 column, by using a simple linear gradient. Mobile phase A was buffer (50 mM KH2PO4) and mobile Phase B was acetonitrile at a flow rate of 1.0 mL/min. The column temperature was kept at 30°C, and the injection volume was 20 μL. All analytes were separated simultaneously at a retention time (tr) of 3.93, 5.84, 7.06, 8.76, and 9.67 min for DPM, DBM, PTM, FSM, and APL, respectively, with a total run time of less than 15.0 min. The proposed method was validated according to ICH guidelines with respect to accuracy, precision, linearity, limit of detection, limit of quantitation, and robustness. Linearity was obtained over a concentration range of 12.0–240.0, 12.0–240.0, 20.0–200.0, 6.0–240.0, and 10.0–200.0 μg/mL DPM, DBM, PTM, FSM, and APL, respectively. Interday and intraday accuracy and precision data were recorded in the acceptable limits. The new method has successfully been applied for quantification of all five drugs in their injection dosage form, infusion samples, and for evaluation of the stability of investigated drugs in mixtures for endovenous use. The results of the stability study showed that mixtures of DPM, DBM, PTM, FSM, and APL in 5% glucose or 0.9% sodium chloride injection were stable for 48 hours when stored in polypropylene syringes at 25°C.

Stability indicating assay method for determination of Febuxostat by RP-HPLC

2021 ◽  
Vol 01 ◽  
Author(s):  
Ramanlal N. Kachave ◽  
Pragati B. Mandlik ◽  
Akshay G. Mundhe
Keyword(s):  
Limit Of Detection ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Photolytic Degradation ◽  
Limit Of Quantitation

Objective: A simple, rapid, precise and accurate RP-HPLC stability indicating method was developed and validated for estimation of Febuxostat in bulk drug and marketed tablet formulation. Methods: The chromatographic separation was achieved on Agilent C18 (250 x 4.6mm, 5 µm) using solvent 15 mM ammonium acetate buffer (pH 4.8) and acetonitrile (30:70 v/v) as a mobile phase at flow rate of 1 mL/min and at ambient column temperature analysis were carried out at detection wavelength 315nm. Result: The method was validated for linearity, precision, accuracy, specificity, LOD and LOQ, and robustness. The linearity was studied in the concentration range of 5-25 µg/mL and correlation coefficient was found to be 0.999. The limit of detection and limit of quantitation were found to be 0.37 µg/mL and 1.13 µg/mL. Febuxostat was subjected to stress condition of degradation including acidic, alkaline, oxidation, photolytic and thermal degradation. Febuxostat is more sensitive toward acidic condition than oxidation and less sensitive towards alkaline, thermal and photolytic degradation. Conclusion: The method is simple, reliable, sensitive and precise which could separate the drug and their degraded product formed under various stress conditions, thus it can be employed as stability indicating method for the determination of FBX in bulk and pharmaceutical dosage form.

Development and Validation of Stability-Indicating HPLC Method for Roflumilast and Related Substances

2013 ◽  
Vol 781-784 ◽  
pp. 68-71 ◽  
Author(s):  
Fang Tan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Related Substances ◽  
Limit Of Quantitation

A reversed phase HPLC method was developed and validated for analysis of roflumilast, its related substances and degradation products, using Ecosil C18 column (250×4.6 mm, 5 μm) with a flow rate of 1.0 ml/min and detection wavelength of 215nm. The mobile phase was a mixture of acetonitrile and 0.005mol·L-1ammonium dihydrogen phosphate buffer pH 3.5 in the ratio of 48:52 (v/v). The samples were analyzed using 20 μl injection volume and the column temperature was maintained at 30°C. The limit of detection and limit of quantitation were found to be 2.6 ng/ml and 8ng/ml, respectively. The stability-indicating capability of method was established by forced degradation studies and method demonstrated successful separation of drug, its related substances and degradation products. The method is sensitive, specific, accurate, precise and stability indicating for the quantitation of drug, its related substances and other degradation compounds.

scholarly journals A Validated RP-HPLC Method for the Determination of Citrinin in Xuezhikang Capsule and otherMonascus-Fermented Products

2012 ◽  
Vol 9 (1) ◽  
pp. 260-266 ◽  
Author(s):  
Li Xue-Mei ◽  
Shen Xing-Hai ◽  
Xue Lan ◽  
Duan Zhen-Wen ◽  
Guo Shu-Ren
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Quantitative Detection ◽  
Rp Hplc ◽  
Toxic Product ◽  
Limit Of Quantitation ◽  
Xuezhikang Capsule ◽  
Fermented Products

Citrinin is a toxic product usually produced during theMonascusfermentation. The presence of citrinin in xuezhikang capsule has been a concern due to its ingredient which is derived frommonascus-fermented rice. A rapid and sensitive RP-HPLC method with fluorescence detection at λex= 331 nm and λem= 500 nm for analysis of citrinin inMonascus-fermented products was developed to analyze citrinin inMonascus-fermented products. The chromatography was performed with mobile phase containing acidified water and acetonitrile. The calibration curve was linear (r = 0.9999) over a range of 0.0107- 0.537 μg/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.187 ng/mL and 0.6 ng/mL respectively. The analysis of xuezhikang capsules using the developed method suggested that the product does not contain detectable citrinin and the result has been further confirmed using independent LC-MS/MS analysis. The proposed method has also been applied to analyze 11 samples of otherMonascus-fermented products. The results suggested that there were no detectable citrinin in 4 of the 11 samples, however citrinin with the levels between 0.10-594 ng/kg has been detected in the other 7 samples. It indicates that the proposed method can also be applied to carry out the quantitative detection of citrinin for otherMonascus-fermented products.

scholarly journals DEVELOPMENT AND VALIDATION OF DAPAGLIFLOZIN BY REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD AND IT’S FORCED DEGRADATION STUDIES

2017 ◽  
Vol 10 (11) ◽  
pp. 101
Author(s):  
Shaik Shakirbasha ◽  
Sravanthi P
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Wave Length ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Column Temperature ◽  
Rp Hplc ◽  
Limit Of Quantitation

  Objective: To develop and validate a simple, selective, precise, and accurate method for the estimation of dapagliflozin using reversed-phase high-performance liquid chromatography (RP-HPLC) technique in bulk and tablet formulation.Methods: The proposed method utilizes chromatographic conditions hypersil BDS (250 mm × 4.6 mm, 5 μ), mobile phase was buffer:acetonitrile (60:40) ratio, flow rate was maintained 1 ml/minute, column temperature was set at 30°C, detection wave length was 245 nm, and diluent was mobile phase.Results: By injecting 5 times of the standard solution system suitability parameters were studied, and results were found well under the acceptance criteria. The linearity study was performed by taking 25-150% levels, and the R2 value was found to be 0.999, precision was found to be 0.5 for repeatability and 0.31 for intermediate precision. The % recovery was found to be 99.89%. Limit of detection and limit of quantitation were found to be 0.60 μg/ml and 1.81 μg/ml, respectively. The % purity was found to be 99.71%. Degradation study on dapagliflozin was performed and concluded that the purity threshold was more than purity angle and within the acceptable range.Conclusion: The developed RP-HPLC method for dapagliflozin was found to be simple, precise, accurate, reproducible, and cost effective. Statistical analysis of the developed method conforms that the proposed method is an appropriate and it can be useful for the routine analysis. This method gives the basic idea to the researcher who is working in area such as product development and finish product testing.

scholarly journals A Validated RP-HPLC Stability Method for the Estimation of Chlorthalidone and Its Process-Related Impurities in an API and Tablet Formulation

2020 ◽  
Vol 2020 ◽  
pp. 1-11
Author(s):  
Chaitali Kharat ◽  
Vaishali A. Shirsat ◽  
Yogita M. Kodgule ◽  
Mandar Kodgule
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Buffer Solution ◽  
Related Impurities ◽  
First Line Therapy ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Bulk Drug ◽  
Simultaneous Identification

Low-dose thiazide and thiazide-like diuretics are widely used as first-line therapy for hypertension. Chlorthalidone, a monosulfamyl diuretic, is frequently prescribed in cases of hypertension and congestive heart failure. In this research paper, an improved reverse-phase HPLC method was developed for the simultaneous identification and quantitation of pharmacopoeia-listed and in-house process- and degradation-related impurities of chlorthalidone in bulk drug and formulations. Chromatographic separation was carried out on a C8 column (250 × 4.6 mm; ‘5 μm particle size) at a flow rate of 1.4 mL/min with a 220 nm detection wavelength. Mobile phase A consisted of buffer solution (diammonium hydrogen orthophosphate (10 mM, pH 5.5)) and methanol at a 65 : 35 ratio (v/v), and mobile phase B consisted of buffer solution and methanol at a 50 : 50 ratio (v/v). The API and formulation were subjected to stress conditions such as acid, alkali, oxidation, thermal, and photolytic conditions. Validation studies for the in-house process impurities were performed for specificity, limit of detection (LOD), limit of quantitation (LOQ), linearity, precision, accuracy, and robustness. Thus, an improved RP-HPLC method capable of good separation of all known and unknown impurities with acceptable resolution and tailing factor was developed.

scholarly journals Ruggedness testing of an HPLC method for the determination of ciprofloxacin

2005 ◽  
Vol 70 (7) ◽  
pp. 979-986 ◽  
Author(s):  
Predrag Sibinovic ◽  
Andreja Smelcerovic ◽  
Radosav Palic ◽  
Sinisa Djordjevic ◽  
Valentina Marinkovic
Keyword(s):  
Aqueous Phase ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Optimal Conditions ◽  
Column Temperature ◽  
Limit Of Quantitation ◽  
Peak Areas ◽  
Ruggedness Testing

The possibility of optimization of an HPLC method for the determinations of ciprofloxacin and ciprofloxacin impurity C was investigated according to the British Pharmacopoeia, using ruggedness testing. Four factors were selected to be tested in this ruggedness test (temperature of the column, volume of acetonitrile in the mobile phase, volume of the aqueous phase in the mobile phase and pH of the aqueous phase in the mobile phase). Seven responses were determined in each design experiment: retention times, peak heights, peak widths, number of theoretical plates, peak areas, peak areas RSD (%) and selectivity. A three-level design was used. The optimal conditions for the chromatographic procedure determined as the result of ruggedness testing were: pH of the aqueous phase in the mobile phase 3.0, column temperature 42 ?C and the acetonitrile to aqueous ratio in the mobile phase 14: 86 (v/v). The HPLC method using the optimal conditions was tested for selectivity linearity, precision, accuracy, limit of quantitation and limit of detection. The applicability of the suggested method was, as well, tested on the stability of ciprofloxacin in pharmaceutical preparations (tablets and infusion solution, products of Zdravlje-Pharmaco, Serbia) under stress stability data.

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