scholarly journals Validated Reversed-Phase Column High-Performance Liquid Chromatographic Method for Separation and Quantification of Polyphenolics and Furocoumarins in Herbal Drugs

2008 ◽  
Vol 91 (5) ◽  
pp. 1020-1024
Author(s):  
Raghavan Govindarajan ◽  
Dhirendra Pratap Singh ◽  
Ajay Kumar Singh Rawat
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Herbal Drugs ◽  
Whole Plant ◽  
Relative Standard ◽  
Different Types ◽  
Photodiode Array ◽  
Almost All ◽  
Liquid Chromatographic

Abstract A rapid column high-performance liquid chromatographic-photodiode array method has been developed for the separation and identification of secondary metabolites, especially different types of phenols and furocoumarins, in a 35 min chromatographic run. The method has been optimized and validated for selectivity, precision, recovery, and robustness with the aim of application for standardization of selected herbal drugs. Almost all of the tested compounds had linearity of >98, with relative standard deviation <10 in terms of variation of retention time. Interday and intraday variability was <5. The developed method has been successfully applied in identification and quantification of phenols and furocoumarins present in different plants, viz., Artemisia pallens (whole plant), Hibiscus rosa-sinensis DC (flower), Heracleum candicans DC (fruit), and Ficus carica Linn (bark). The results indicate that the method is rapid, accurate, and robust for the analysis of different types of phenols and furocoumarins and, hence, can be successfully used in the quality control and standardization of plant extracts and herbal drugs.

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 Simple and Rapid Liquid Chromatography Method for Determination of Rifabutin in Plasma

2013 ◽  
Vol 9 (2) ◽  
pp. 26-29 ◽  
Author(s):  
AK Hemanth Kumar ◽  
V Sudha ◽  
Geetha Ramachandran
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Pharmacokinetic Studies ◽  
Chromatography Method ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatography Method ◽  
Liquid Chromatographic

A high performance liquid chromatographic method for determination of rifabutin in human plasma was  developed. The method involved deproteinisation of the sample with acetonitrile and analysis of the  supernatant using a reversed-phase C18 column (250mm) and UV detection at a wavelength of 265nm.  The assay was specific for rifabutin and linear from 0.025 to 10.0μg/ml. The relative standard deviation  of intra- and inter-day assays was lower than 10%. The method was able to remove interfering materials  in plasma, yielding an average recovery of rifabutin from plasma of 101%. Due to its simplicity, the assay  can be used for pharmacokinetic studies of rifabutin. SAARC Journal of Tuberculosis, Lung Diseases & HIV/AIDS; 2012; IX(2) 26-29 DOI: http://dx.doi.org/10.3126/saarctb.v9i2.7975

scholarly journals Quantitation of Sitagliptin in Drug Product by Validated Reversed Phase Liquid Chromatographic Technique

2018 ◽  
Vol 17 (1) ◽  
pp. 123-129
Author(s):  
Sharifa Sultana ◽  
Md Shahadat Hossain ◽  
Md Samiul Islam ◽  
Abu Shara Shamsur Rouf
Keyword(s):  
High Performance ◽  
Drug Product ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Chromatographic Technique ◽  
Pharmaceutical Dosage Form ◽  
Relative Standard ◽  
Liquid Chromatographic

A novel reversed phase ultra-high performance liquid chromatographic (RP-UHPLC) method was developed for the estimation of sitagliptin in pharmaceutical dosage form. Separation was done by a X-bridge C18 column (4.6 i.d.× 150 mm, 5 μm particle size) with a flow rate of 1 ml/min using phosphate buffer (pH 6) and acetonitrile (70:30, v/v) as mobile phase at 268 nm using photodiode array plus (PDA+) detector. The retention time was found at 4.607 min. The developed method was validated as per the requirements of ICH-Q2B guidelines for specificity, system suitability, linearity, precision, accuracy, sensitivity and robustness. The linear regression analysis data for the linearity plot showed correlation coefficient values of 0.999 with LOD value of 0.06 μg/ml and LOQ of 0.225 μg/ml. The relative standard deviation (%RSD) for inter-day and intra- day precision was not more than 2.0%. The method was found to be accurate with percentages recovery of 98.50±0.03 to 99.70±0.05 and the % RSD was less than 2. The results showed that the proposed method is highly convenient for routine analysis of sitagliptin.Dhaka Univ. J. Pharm. Sci. 17(1): 123-129, 2018 (June)

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.

scholarly journals Column High-Performance Liquid Chromatographic Determination of Norfloxacin and Its Main Impurities in Pharmaceuticals

2008 ◽  
Vol 91 (2) ◽  
pp. 332-338 ◽  
Author(s):  
Branislava Mielji ◽  
Gordana Popovi ◽  
Danica Agbaba ◽  
Slavko Markovi ◽  
Breda Simonovska ◽  
...  
Keyword(s):  
High Performance ◽  
Raw Materials ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Array Detector ◽  
Chromatographic Separations ◽  
Experimental Conditions ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A gradient reversed-phase column high-performance liquid chromatographic method was developed for the detection and quantification of norfloxacin and its major impurities in norfloxacin-containing pharmaceuticals. Chromatographic separations were performed under the following experimental conditions: column, Zorbax SB RP-18 (5 m, 250 4.6 mm); injection volume, 20 L; mobile phase, 0.05 M NaH2PO4 (pH 2.5)acetonitrile (87 + 13) for 16 min and (58 + 42) for 9 min (stepwise gradient); and flow rate, 1.3 mL/min. All analyses were performed at 25C, and the eluate was monitored at 275 nm using a diode array detector. Linearity (correlation coefficient = 0.999), recovery (99.3101.8), relative standard deviation (0.20.7), and quantitation limit (0.120.47 g/mL) were evaluated and found to be satisfactory. The method is simple, rapid, and convenient for purity control of norfloxacin in both raw materials and dosage forms.

scholarly journals Simultaneous Determination of Six Major Constituents of the Herbal Formula Insampaedok-san Using HPLC-PDA

2012 ◽  
Vol 2012 ◽  
pp. 1-6 ◽  
Author(s):  
Chang-Seob Seo ◽  
Jung Hoon Kim ◽  
Hyeun-Kyoo Shin
Keyword(s):  
Acetic Acid ◽  
High Performance ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Aqueous Acetic Acid ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Photodiode Array ◽  
Liquid Chromatographic

A simple, rapid, and accurate high-performance liquid chromatographic method was applied to the quantitative analysis of six components of a traditional herbal formulation, Insampaedok-san (ISPDS): liquiritin (1), ferulic acid (2), naringin (3), hesperidin (4), neohesperidin (5), and glycyrrhizin (6). The six components were separated within 35 min using a Gemini C18 column maintained at 40°C. The mobile phase was composed of 1.0% (v/v) aqueous acetic acid (A) and 1.0% (v/v) acetic acid in acetonitrile (B) by gradient elution. The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 254, 280, and 320 nm. The calibration curves showed good linearity (R2=1.0000) for different concentration ranges. The recovery of each component was in the range of 92.62%–105.96%, with a relative standard deviation (RSD) of less than 4.0%. The RSDs for intra- and interday precision were 0.04%–1.70% and 0.06%–2.56%, respectively. The concentration of each of the six components of ISPDS was in the range 0.72–9.88 mg g−1.

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 DETERMINATION OF 5H-BENZO[2,3][1,4]OXAZEPINO[5,6-B]INDOLES IN RAT PLASMA BY REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC-ULTRAVIOLET METHOD: APPLICATION TO PHARMACOKINETIC STUDIES

2017 ◽  
Vol 10 (12) ◽  
pp. 425 ◽  
Author(s):  
Ashok K Singh ◽  
Vinit Raj ◽  
Amit Rai ◽  
Amit K Keshari ◽  
Pranesh Kumar ◽  
...  
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Rat Plasma ◽  
Reversed Phase ◽  
Pharmacokinetic Studies ◽  
Relative Standard ◽  
Liquid Chromatographic

Objective: Recently, we reported newly synthesized 5H-benzo[2,3][1,4]oxazepino[5,6-b]indole) derivatives and proved their cytotoxicity against hepatocellular carcinoma specific Hep-G2 cell lines. We attempted herein to describe a reversed-phase high-performance liquid chromatographic method for the determination of three most active compounds 6a, 10a, and 15a in rat plasma to predict their pharmacokinetics parameters before in vivo study.Methods: A rapid and sensitive reversed-phase high-performance liquid chromatographic was employed for the determination of 6a, 10a, and 15a in rat plasma. Each compound was separated by a gradient elution of acetonitrile and water with 1 mL/min flow rate. The detector was set at 270, 285, and 275 nm for 6a, 10a, and 15a and the recorded elution times were 2.00, 2.87, and 1.88 min, respectively.Results: The calibration curve was linear with R2 of 0.938, 0.875, and 0.923 over the concentration range of 0.1–50 μg/mL. The inter- and intra-day variations of the assay were lower than 12.26%; the average recovery of 6a, 10a, and 15a was 97.31, 92.56, and 95.23 % with relative standard deviation of 2.12%, 3.25%, and 2.28%, respectively. The Cmax and Tmax were ~ 46.34, 18.56, and 25.65 μg/mL and 2.0, 4.0, and 4.0 h for 6a, 10a, and 15a, respectively, which indicate a robust method of detection in the present experiment.Conclusion: The study suggests that all of the three compounds have a lower rate of absorption, higher volume of distribution, and lower clearance rate, indicating good therapeutic response for in vivo activity. 

scholarly journals Simultaneous Determination of Phenolic Acids and Phthalide Compounds by Liquid Chromatography for Quality Assessment of Rhizoma Cnidii

2009 ◽  
Vol 92 (2) ◽  
pp. 375-381
Author(s):  
M Nurul Islam ◽  
Hye Hyun Yoo ◽  
Chung-Ki Sung ◽  
Mi-Sook Dong ◽  
Young In Park ◽  
...  
Keyword(s):  
Ferulic Acid ◽  
Chlorogenic Acid ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Bioactive Constituents ◽  
Linear Behavior ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract This paper describes a simple, rapid, and validated reversed-phase high-performance liquid chromatographic method developed for the determination of 4 major bioactive constituents, namely, chlorogenic acid, ferulic acid, senkyunolide A, and Z-ligustilide in Rhizoma Cnidii extract. A Capcell Pak C18 chromatographic column (150 4.6 mm, 3 m) was used with mobile phases consisting of 0.1 formic acid, acetonitrile, and methanol at a flow rate of 0.8 mL/min and UV detection at 285 nm. Comprehensive validation of the method included evaluation of linearity, repeatability, recovery, and stability. Excellent linear behavior (r2 >0.99) was observed over the concentration range of 2100 g/mL for the compounds under investigation. Repeatability and accuracy were evaluated by intra- and interday assays; the relative standard deviation (RSD) values were 5.37 and accuracies ranged from 97.1 to 104.9. Recoveries of the compounds ranged from 94.2 to 104.2 with RSD values of 9.50. The developed method was successfully applied to the analysis of ethanolic extracts of Rhizoma Cnidii samples. As a result, the concentrations of chlorogenic acid, ferulic acid, Z-ligustilide, and senkyunolide A were determined to be 0.845.35, 0.451.65, 0.744.39, and 0.321.14 mg/g herb, respectively. Thus, the developed method was found to be accurate and reproducible and is considered suitable for the qualitative and quantitative analysis of Rhizoma Cnidii for bioactive compounds.

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