scholarly journals A Simple Analytical Method for High-Throughput Screening of Major Sugars from Soybean by Normal-Phase HPLC with Evaporative Light Scattering Detection

2015 ◽  
Vol 2015 ◽  
pp. 1-8 ◽  
Author(s):  
Babu Valliyodan ◽  
Haiying Shi ◽  
Henry T. Nguyen
Keyword(s):  
Light Scattering ◽  
Analytical Method ◽  
High Throughput Screening ◽  
Mobile Phase ◽  
High Performance ◽  
Pure Water ◽  
Gradient Elution ◽  
Chromatographic Retention ◽  
Simple Analytical Method ◽  
Evaporative Light Scattering

This paper presents a simple analytical method for determining sugars in soybean (Glycine max (L.) Merr.) tissues. Sample preparation was modified from several early published methods. High-performance liquid chromatography (HPLC) equipped with an evaporative light scattering detector (ELSD) was used to separate, identify, and quantify seven sugars, including glucose, galactose, fructose, sucrose, melibiose, raffinose, and stachyose. Two mobile phases were programed into a gradient elution. Mobile phase A is pure water and mobile phase B is a mixture of acetonitrile and acetone 75 : 25 (v/v). Total chromatographic retention time is less than 20 minutes. This method has been validated for detection limit, calibration range, and intraday and interday repeatability. This method has been used analyzing more than 5000 soybean samples in the experiments studying natural genetic variation of sugar contents and components in soybean seeds and other tissues.

scholarly journals Identification and Quantification of three Tubeimosides in Rhizoma Bolbostematis by High Performance Liquid Chromatography with Evaporative Light Scattering Detection and Electrospray Mass Spectrometric Detection

2008 ◽  
Vol 3 (5) ◽  
pp. 1934578X0800300 ◽  
Author(s):  
Hao Huang ◽  
MingJin Liang ◽  
Wen Xu ◽  
Chuan Zhang ◽  
WeiDong Zhang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Light Scattering ◽  
High Performance ◽  
Methanol Extract ◽  
Gradient Elution ◽  
Evaporative Light Scattering Detection ◽  
Light Scattering Detection ◽  
Evaporative Light Scattering

Tubeimoside I, tubeimoside II and tubeimoside III were simultaneously determined and identified by high performance liquid chromatography coupled with electrospray tandem mass spectrometry (HPLC-ESI/MS), and a novel and sensitive high performance liquid chromatography - evaporative light scattering detection (HPLC-ELSD) in a 70% methanol extract of Rhizoma Bolbostematis. The chromatographic separation was performed on a Zorbax Extend C18 analytical column using gradient elution with a solution of acetonitrile and 0.5% acetic acid. The method was validated with acceptable linearities (r > 0.9992) and recoveries (98.6 to 102.4 %). The limits of detection of these three tubeimosides were as low as 0.05 μg. The intra- and inter-day precisions of the method were evaluated and were less than 3.6%. The method was successfully used to analyze 15 batches of Rhizoma Bolbostematis. The content of tubeimosides in the plant material varied from habitat to habitat confirming the necessity to control the quality of Rhizoma Bolbostematis during its preparation and application in the clinic.

scholarly journals A NOVEL ANALYTICAL METHOD FOR SIMULTANEOUS QUANTIFICATION OF DAPAGLIFLOZIN AND SITAGLIPTIN BY REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2021 ◽  
Vol 10 (3) ◽  
pp. 2861-2865
Author(s):  
Ajay Gupta
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
High Performance ◽  
Potassium Phosphate ◽  
Cost Effective ◽  
Gradient Elution ◽  
Hplc Method ◽  
Reverse Phase ◽  
Simultaneous Quantification ◽  
Validation Parameters

The Reverse phase HPLC method was developed for simultaneous determination of Dapagliflozin and Sitagliptin in single analytical method. Chromatographic separation was achieved on a Hypersil BDS C18 (250mmx4.6mm, 5µm) column applying an gradient elution based on potassium phosphate monobasic buffer pH (3.0) as mobile phase A while methanol and acetonitrile in the ratio of (60:40 v/v) as a mobile phase B with gradient program Time/Mobile phase A%/Mobile phase B% is as 0 min./55/45, 3 min./55/45, 9 min./20/80, 13 min.20/80, 15 min./55/45, 20 min./55/45. Validation parameters specificity, linearity, accuracy, precision and robustness have been observed to be desirable over the concentration ranges of 50-150 µg/ml for Dapagliflozin and Sitagliptin respectively. All the variables have been studied to optimize the chromatographic conditions. The optimized approach verified through validation and confirmed to be the intended purpose for the quality control of the mentioned drugs, as per ICH guidelines. For simultaneous quantification of Dapagliflozin and Sitagliptin, the developed method was found to be genuinely exact precise, accurate, linear, fast, and cost effective.

Analysis of organic impurities of besifloxacin hydrochloride by high performance liquid chromatography with isocratic and gradient elution.

2019 ◽  
Vol 16 ◽  
Author(s):  
Joanna Wittckind Manoel ◽  
Camila Ferrazza Alves Giordani ◽  
Livia Maronesi Bueno ◽  
Sarah Chagas Campanharo ◽  
Elfrides Eva Sherman Schapoval ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Gradient Elution ◽  
Pharmaceutical Product ◽  
Raw Material ◽  
Isocratic Elution ◽  
Organic Impurities ◽  
Elution Method

Introduction: Impurity analysis is an important step in the quality control of pharmaceutical ingredients and final product. Impurities can arise from drug synthesis or excipients and even at small concentrations may affect product efficacy and safety. In this work two methods using high performance liquid chromatography (HPLC) were developed and validated for the evaluation of besifloxacin and its impurity synthesis, with isocratic elution and another with gradient elution. Method: The analysis by HPLC in isocratic elution mode was performed using a cyano column maintained at 25 °C. The mobile phase was composed by 0.5% triethylamine (pH 3.0): acetonitrile (88:12 v/v) eluted at a flow rate of 1.0 ml/min with detection at 330 nm. The gradient elution method was carried out with the same column and mobile phase components only modifying the rate between organic and aqueous phase during analysis. The procedures have been validated according to internationally accepted guidelines, observing results within acceptable limits. Results: The methods presented were found to be linear in the 140 to 260 µg/ml range for besifloxacin and 0.3 to 2.3 µg/ml for an impurity named A. The limits of detection and quantification were respectively 0.07 and 0.3 µg/ml for impurity A, with a 20 µL injection volume. The precision achieved for all analyses performed provided RSD inter-day equal to 6.47 and 6.36% for impurity A with isocratic elution and gradient, respectively. The accuracy was higher than 99% and robustness exhibited satisfactory results. In the isocratic method an analysis time of 25 min and 15 min was obtained for gradient. For impurity A, the number of theoretical plates in the isocratic mode was about 5000 while in the gradient mode it was about 45000, hence, it made the column more efficient by changing the mobile phase composition during elution. In besifloxacin raw material and in pharmaceutical product used in this study, other related impurities were present but but impurity A was searched for and not detected Conclusion: The proposed methods can be applied for quantitative determination of impurities in the analysis of the besifloxacin raw material, as well as in ophthalmic suspension of the drug, considering the quantitation limit.

scholarly journals Determination of Triterpenoids and Phenolic Acids from Sanguisorba officinalis L. by HPLC-ELSD and Its Application

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4505
Author(s):  
Jiahui Sun ◽  
Chunli Gan ◽  
Jing Huang ◽  
Zhenyue Wang ◽  
Chengcui Wu ◽  
...  
Keyword(s):  
Phenolic Acids ◽  
High Performance ◽  
Gradient Elution ◽  
Light Scattering Detection ◽  
Evaporative Light Scattering ◽  
Acetic Acid Water ◽  
Sanguisorba Officinalis ◽  
Functional Components ◽  
Gradient Elution Mode

A novel analytical method involving high-performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD) was developed for simultaneous determination of 11 phenolic acids and 12 triterpenes in Sanguisorba officinalis L. Chromatographic separation was conducted with gradient elution mode by using a DiamonsilTM C18 column (250 mm × 4.6 mm, 5 μm) with the mobile phase of 0.1% acetic acid water (A) and methanol (B). The drift tube temperature of ELSD was set at 70 °C and the nitrogen cumulative flow rate was 1.6 L/min. The method was fully validated to be linear over a wide concentration range (R2 ≥ 0.9991). The precisions (RSD) were less than 3.0% and the recoveries were between 97.7% and 101.4% for all compounds. The results indicated that this method is accurate and effective for the determination of 23 functional components in Sanguisorba officinalis L. and could also be successfully applied to study the influence of processing method on those functional components in Sanguisorba officinalis L.

scholarly journals Gradient HPLC in the determination of drug lipophilicity and acidity

2001 ◽  
Vol 73 (9) ◽  
pp. 1465-1475 ◽  
Author(s):  
Roman Kaliszan ◽  
Piotr Haber ◽  
Tomasz Baczek ◽  
Danuta Siluk
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Standard Procedure ◽  
Gradient Elution ◽  
Log P ◽  
Retention Data ◽  
Organic Modifier ◽  
Wide Range ◽  
Aqueous Component ◽  
Initial Ph

The linear-solvent strength (LSS) model of gradient elution in high-performance liquid chromatography (HPLC) has been demonstrated to provide parameters of lipophilicity and acidity of analytes. pKa and log kw values are determined in three gradient runs. The first two experiments use an aqueous buffered eluent with a wide-range organic modifier gradient at pH of buffer, providing suppression of ionization of the analyte. That experiment allows an estimate of contents of the organic modifier in the mobile phase (%B), producing requested retention coefficient, k, for the nonionized form of the analyte. The next experiment is carried out with the latter %B and a pH-gradient of the aqueous component of the eluent that is sufficient to overlap possible pKa value of the analyte. The initial pH of the buffer used to make the mobile phase is selected to insure that the analyte is in nonionized form. The resulting retention time allows an estimate of pKa in a solvent of the given %B.The log kw parameter obtained correlated well with the corresponding value obtained by the standard procedure of extrapolation of retention data determined in a series of isocratic measurements. The correlation between log kw and the reference parameter of lipophilicity, log P, was very good for a series of test analytes. The values of pKa were found to correlate with the literature pKa data determined in water for a set of aniline derivatives studied.

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