Analysis of spectinomycin in fermentation broth by reversed-phase chromatography

2009 ◽  
Vol 63 (6) ◽  
Author(s):  
Hong Yan ◽  
Pei Xu ◽  
Hai Huang ◽  
Juan Qiu
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Fermentation Broth ◽  
Correlation Coefficients ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Standard Curve ◽  
Relative Standard ◽  
Liquid Chromatographic

AbstractA pre-column derivatized high-performance liquid chromatographic (HPLC) method with ultraviolet-visible detection was developed to measure the concentrations of spectinomycin in fermentation broth. Derivatization reagents, 2,4-dinitrophenylhydrazine in acetonitrile (5 mg mL−1) and trifluoroacetic acid in acetonitrile (0.8 mol L−1), were added to an aliquot of the fermentation broth, and the mixture was incubated for 60 min at 70°C. The resulting derivative was separated from other compounds by isocratic elution in a reversed-phase column Zorbax SB-C18 (250 mm × 4.6 mm, 5 µm). Mobile phase consisted of acetonitrile, tetrahydrofuran, and water (φ r = 40: 35: 25) and the flow rate was 1.0 mL min−1. The detection wavelength was 415 nm. The standard curve for spectinomycin sulfate was linear with correlation coefficients of 0.9997 in the range of 25 µg mL−1 to 600 µg mL−1. The relative standard deviation values ranged from 0.43 % to 2.18 % depending on the concentration of samples. The average recovery was 101.5 %. The limit of detection was 50 ng mL−1.

DEVELOPMENT OF VALIDATED RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF CHROMIUM PICOLINATE III IN A DIET VINEGAR FORMULATION

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 48-52
Author(s):  
A Lodhi ◽  
◽  
A Jain ◽  
B. Biswal
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Chromium Picolinate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A validated high performance liquid chromatographic method was developed for the determination of chromium picolinate in pharmaceutical dosage forms. The analysis was performed at room temperature using a reversed-phase ODS, 5µm (250×4.6) mm column. The mobile phase consisted of acetonitrile: buffer (60:40 V/V) at a flow rate of 0.5 mL/min. The PDA-detector was set at 264 nm. The developed method showed a good linear relationship in the concentration range from 1.5 – 12.5 µg/mL with a correlation coefficient from 0.999. The limit of detection and limit of quantification were 0.0540513 and 0.1637919 µg/mL respectively.

scholarly journals Development of a New High-Performance Liquid Chromatographic Method for the Determination of Ceftazidime

2008 ◽  
Vol 91 (4) ◽  
pp. 739-743 ◽  
Author(s):  
Andréia de Haro Moreno ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Calibration Graph ◽  
Raw Material ◽  
Relative Standard ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanolwater (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 g/mL. The values for interday and intraday precision (relative standard deviation) were <1. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.

scholarly journals Development and Validation of a RP-HPLC Method for the Estimation of Amlexanox in Oral Paste Dosage Form

2012 ◽  
Vol 10 (2) ◽  
pp. 67-70
Author(s):  
Abdullah Al Masud ◽  
Mohammad Saydur Rahman ◽  
Towfika Islam ◽  
Saki Sultana ◽  
Moynul Hasan ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Dynamic Range ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic

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

Development of RP-HPLC Method for Estimation of Valsartan and Hydrochlorothiazide in Tablets

2013 ◽  
Vol 6 (4) ◽  
pp. 2240-2244
Author(s):  
Cylma Menezes ◽  
Vishal M ◽  
Shyamkumar B ◽  
Reema N
Keyword(s):  
High Performance ◽  
Dynamic Range ◽  
Correlation Coefficients ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Liquid Chromatographic

A simple, efficient and reproducible reversed phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the simultaneous estimation of valsartan and hydrochlorothiazide in bulk and in tablets. A column having 250 x 4.6 mm i.d. (Kromasil C18) in isocratic mode with mobile phase containing 50 mM potassium dihydrogen o-phosphate buffer (triethylamine 0.2%), (pH 3.7 adjusted with o-phosphoric acid): acetonitrile (56:44 v/v) was used. The flow rate was 1.0 ml/min and effluent was monitored at 232 nm.  The retention time of valsartan and hydrochlorothiazide was 10.15 and 3.78 min respectively. All calibration curves showed good linear correlation coefficients within the tested limits (r2 > 0.9995). The linearity dynamic range was found to be 20-150 µg/ml and 5-45 µg/ml for valsartan and hydrochlorothiazide respectively. Percentage recoveries for valsartan and Hydrochlorothiazide were 100.45 % and 98.75 % respectively. All the analytical validation parameters were determined and found in the limit as per the International Conference on Harmonization (ICH) guidelines which indicates the validity of the method. The developed method was found to be accurate, precise and robust for the simultaneous estimation of valsartan and hydrochlorothiazide in bulk and in tablets.

scholarly journals Development and Validation of Column High-Performance Liquid Chromatographic and Ultraviolet Spectrophotometric Methods for Citalopram in Tablets

2008 ◽  
Vol 91 (1) ◽  
pp. 52-58 ◽  
Author(s):  
Jlia Menegola ◽  
Martin Steppe ◽  
Elfrides E S Schapoval
Keyword(s):  
Spectrophotometric Method ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Significant Difference ◽  
Liquid Chromatographic

Abstract Column high-performance liquid chromatographic (LC) and UV spectrophotometric methods for the quantitative determination of citalopram, a potent and selective serotonin reuptake inhibitor, in tablets were developed. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection, and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by the reversed-phase technique on an ACE C18 column with a mobile phase composed of 0.30 triethylamine solutionacetonitrile (55 + 45, v/v) adjusted to pH 6.6 with 10 ortho-phosphoric acid at a flow rate of 1.0 mL/min and 25C. The UV spectrophotometric method was performed at 239 nm. The linearity of the LC method was in the range of 10.0070.00 g/mL, and 2.5017.50 g/mL for the UV spectrophotometric method. The interday and intraday assay precision was <1.5 (relative standard deviation) for the LC and UV spectrophotometric methods. The recoveries were in the range 100.70101.35 for the LC method and 98.4898.65 for the UV spectrophotometric method. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the 2 methods. The proposed methods are highly sensitive, precise, and accurate and can be used for the reliable quantitation of citalopram in tablets.

scholarly journals Development of Simple and Robust RP-HPLC Method for Determination of Everolimus and its Impurities in Oral Solid Dosage Form

2019 ◽  
Vol 31 (5) ◽  
pp. 1002-1008
Author(s):  
Somana Siva Prasad ◽  
G.V. Krishna Mohan ◽  
A. Naga Babu
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantitation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A novel reversed-phase high performance liquid chromatographic (HPLC) technique for the determination of everolimus (Isomer-B) and its impurities in the tablet dosage form has been optimized using analytical quality by design (QbD) approach. All the compounds are monitored with the photodiode array (PDA) detector at 280 nm and the parameters namely; precision, accuracy, specificity, stability, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The quantitation limits of IMP-A, IMP-B, IMP-C, IMP-D, IMP-E, Sirolimus and TGR are found to be 0.08, 0.08, 0.10, 0.10, 0.10, 0.08 and 0.08, respectively. Recovery studies from 0.9 mg/L to 9.0 mg/L are performed for all impurities and the values were obtained between 85-110 %. Injection volume and test concentrations have been optimized to achieve LOQ values under the reporting threshold. The whole technique is developed and validated as per International Council for Harmonization (ICH) guidelines. The proposed method is robust, sensitive, rapid and successful and helpful in the regions where regulatory agencies recommend HPLC analytical method.

scholarly journals Validated RP-HPLC Method for Analysis of Aripiprazole in a Formulation

2010 ◽  
Vol 7 (3) ◽  
pp. 827-832 ◽  
Author(s):  
R. Kalaichelvi ◽  
B. Thangabalan ◽  
D. Srinivasa Rao
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Rp Hplc ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A rapid, simple and validated reversed-phase high-performance liquid chromatographic method has been developed for analysis of aripiprazole in tablet dosage form. Aripiprazole was separated on an ODS analytical column with a 40:60 (v/v) mixture of acetonitrile and triethanolamine buffer (5 mM, pH 3.5 ± 0.05 adjusted by addition of 85% phosphoric acid) as mobile phase at a flow rate of 1.5 mL min-1. The effluent was monitored by UV detection at 254 nm. Calibration plots were linear in the range of 20 to 60 µg mL-1and the LOD and LOQ were 0.411 and 1.248 µg mL-1, respectively. The high recovery and low relative standard deviation confirm the suitability of the method for routine quality control determination of aripiprazole in tablets.

scholarly journals Development and Validation of Bioanalytical HPLC Method For Estimation of Telmisartan In Rat Plasma: Application To Pharmacokinetic Studies

2013 ◽  
Vol 11 (2) ◽  
pp. 121-127 ◽  
Author(s):  
Jaydeep M Patel ◽  
Anjali P Dhingani ◽  
Kevin C Garala ◽  
Mihir K Raval ◽  
Navin R Sheth
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Rat Plasma ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmacokinetic Parameters ◽  
Pharmacokinetic Studies ◽  
Limit Of Quantification ◽  
Liquid Chromatographic

A simple, specific, sensitive and rapid reversed phase high performance liquid chromatographic (HPLC) method has been developed and validated for the determination of telmisartan in small volumes of rat plasma. Biological sample preparation involving simple extraction with organic solvent, followed by dilution with mobile phase was adopted to eliminate any chromatographic solvent effects. The method was proven to be linear over a plasma concentration range of 10 to 1000 ng/mL with a mean correlation coefficient of 0.9942. The limit of detection and the limit of quantification of the newly developed method were determined to be 1 ng/mL and 10 ng/mL, respectively. The method was successfully applied to assess pharmacokinetic parameters of telmisartan in Wister rats following a single oral dose (1.8 mg/kg, b.w.). The developed method was established as a rapid analytical tool in a pharmacokinetic study as it required short retention time, high precision, sensitivity and small volumes of plasma for analysis. DOI: http://dx.doi.org/10.3329/dujps.v11i2.14562 Dhaka Univ. J. Pharm. Sci. 11(2): 121-127, 2012 (December)

scholarly journals High-performance liquid chromatographic detection of selected phenolic acidsin wine

2021 ◽  
Vol 9 (2) ◽  
Author(s):  
Darinka Brodnjak Vončina ◽  
Maša Islamčivic Razboršek ◽  
Marjana Simonič
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Correlation Coefficients ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Reversed Phase Hplc ◽  
Limit Of Quantitation ◽  
Chromatographic Detection ◽  
Liquid Chromatographic

The aim of this study was to develop a method for identification and quantification of phenolic acids in different wine samples. The simple reversed-phase HPLC-UV method for simultaneous determination of p-coumaric and ferulic acid was developed. The method was validated and working range, linearity, repeatability, accuracy, limit of quantitation LOQ and limit of detection LOD were determined. The linearity of the method was tested in concentration ranges 0.1-1 mg L-1 and 1-10 mg L-1. The correlation coefficients (r2) were greater than 0.996 and quality coefficients (QC) ≤ 5%. Detection limit for both compounds was 0.01 mg L-1. The method is precise (RSD

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

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