scholarly journals Qualitative and Quantitative Analysis of the Main Constituents of Radix Ilicis Pubescentis by LC-Coupled with DAD and ESIMS Detection

2010 ◽  
Vol 5 (1) ◽  
pp. 1934578X1000500 ◽  
Author(s):  
Wen-Yuan Liu ◽  
Feng Feng ◽  
Cheng-Xia Yu ◽  
Ning Xie
Keyword(s):  
Quantitative Analysis ◽  
High Performance ◽  
Southern China ◽  
Accurate Determination ◽  
Extraction Procedure ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Array Detector ◽  
Phase Detection

A sensitive and selective high performance liquid chromatographic method coupled with DAD detection is presented for quality control of Radix Ilicis Pubescentis. By means of this analytical procedure the major individual constituents (ilexoside O, ilexgenin A, ilexsaponin A1, ilexsaponin B1, liriodendin and acanthoside B) could be quantified simultaneously. LC-ESIMS was applied for identification of the six compounds in the plant by comparing their m/z value and retention times with those of selected standards. For quantitative analysis, the extraction procedure and the extraction solvent were optimized in order to ensure the exhaustive extraction of the plant material. The HPLC conditions were evaluated and optimized for the exact quantification of all six individual compounds. Chromatographic separation was carried out on a C18 column using gradient elution with acetonitrile and 0.1% phosphoric acid as the mobile phase. Detection was carried out using a photodiode array detector. The calibration curves for determination of the six constituents showed good linearity over the investigated ranges (r2>0.999). Measurement of intra-day and inter-day variability (expressed as RSD value) was conducted to assess precisions of the method, and RSD (%) of intra- and inter-day variation were between 1.56-3.36% and 1.61-3.58%, respectively. The recoveries of the six compounds were between 96.4-102.2%, with RSD (%) values ranging from 1.7-3.8%. These validation results demonstrated the suitability of the method for the precise and accurate determination of the main constituents in Radix Ilicis Pubescentis. The method was successfully applied for quality evaluation of 12 batches of Radix Ilicis Pubescentis obtained from different regions of southern China. The contents of the six major constituents varied significantly due to their different origins, which can be used as an aid to assessing the quality of Radix Ilicis Pubescentis.

scholarly journals A comparative study of HPLC-DAD and UPLC-UV methods for simultaneous determination of 11 polyphenols in Moringa oleifera leaves

2021 ◽  
Vol 20 (11) ◽  
pp. 2371-2379
Author(s):  
Yanqin Zhu ◽  
Qinhong Yin ◽  
Yaling Yang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Moringa Oleifera ◽  
Accurate Determination ◽  
Gradient Elution ◽  
Hplc Method ◽  
Array Detector ◽  
Moringa Oleifera Leaves

Purpose: To develop, validate and compare two chromatographic methods - high performance liquid chromatography with diode array detector ((HPLC-DAD) and high performance liquid chromatography with ultraviolet detection (UPLC-UV) for the effective analysis of polyphenols in Moringa oleifera leaves.Methods: HPLC-DAD and UPLC-UV methods were applied for the accurate determination of eleven major polyphenols in Moringa oleifera leaves. The chromatographic conditions of the eleven polyphenols was determined on two C18 column by gradient elution with 0.5 % phosphoric acid solution -acetonitrile as the eluate, and at a flow rate of 1.0 and 0.5 mL/min for HPLC-DAD and UPLC-UV methods, respectively. Detector parameter of UPLC-UV was fixed at 203 nm. The assay methods were validated systematically.Results: The instrumental methods (HPLC-DAD and UPLC-UV) had good linearity, precision,repeatability and recovery. For both methods, quantification limits of UPLC-UV (0.057 - 0.363 μg/mL) were lower than those of UPLC-UV (0.094 - 1.532 μg/mL). The UPLC method with a shorter running time and more sensitive detection was applied in comparing to the HPLC method. After optimization and evaluation, the baseline of 11 compounds was separated effectively within 68 and 34 min, respectively.Conclusion: The developed HPLC-DAD and UPLC-UV assays were successfully utilized for thesimultaneous analysis of eleven major polyphenols and can readily be utilized as quality control tools for Moringa oleifera leaves in China, with UPLC-UV method showing better separation, lower organic solvent usage and shorter analytical period.

A Novel HPLC Method for Simultaneous Determination of Methyl, Ethyl, n-propyl, Isopropyl, n-butyl, Isobutyl and Benzyl Paraben in Pharmaceuticals and Cosmetics

2020 ◽  
Vol 23 ◽  
Author(s):  
Saniye Özcan ◽  
Serkan Levent ◽  
Nafiz Öncü Can
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Array Detector ◽  
Methyl Ethyl ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Liquid Chromatographic

: The alkyl esters of p-hydroxybenzoic acid at the C-4 position, “the parabens,” including methyl, ethyl, propyl, and butyl, are widely used as antimicrobial preservatives in foods, cosmetics, and pharmaceuticals. Official regulations on the use of these compounds make their analysis essential for the estimation of their exposure. On this basis, the presented study was realized to develop a simple, selective and cheap high-performance liquid chromatographic method for the quantitative determination of methyl paraben (MP), ethyl paraben (EP), n-propyl paraben (NPP), isopropyl paraben (IPP), n-butyl paraben (NBP), isobutyl paraben (IBP) and benzyl paraben (BP) in pharmaceuticals and cosmetic products. The chromatographic separation of the analytes was achieved under flow rate gradient elution conditions using a C18-bonded core-shell silica particle column (2.6 μm particle size, 150 × 3.0 mm from Phenomenex Co.). The samples were injected into the system as aliquots of 1.0 μL, and the compounds were detected by using a photodiode array detector set at 254 nm wavelength. With this technique, seven paraben derivatives can be determined in the concentration range of 250-2000 ng/mL. The recovery of the method is in the range of 99.95-13.84%, and the RSD is at a maximum value of 3.95%. The proposed method was fully validated and successfully applied to different pharmaceutical and cosmetic samples (n=16), including syrups, suspensions, oral sprays, gels, etc. At least one paraben derivative was detected in six of the samples, and was determined quantitatively. The maximum amount of a paraben derivative found in the analyzed samples is 321.7 ng/mL, which was MP. To the best of our knowledge, this is the first LC method, which is applicable both on pharmaceutical and cosmetic samples.

scholarly journals Rapid determination of theaflavins by HPLC with a new monolithic column

2019 ◽  
Vol 37 (No. 2) ◽  
pp. 112-119 ◽  
Author(s):  
Jianyong Zhang ◽  
Hongchun Cui ◽  
Heyuan Jiang ◽  
Lei Fang ◽  
Weiwei Wang ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Mobile Phase ◽  
High Performance ◽  
Rapid Determination ◽  
Monolithic Column ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
New Strategy

The quantitative determination of four theaflavin monomers by a rapid reversed-phase high performance liquid chromatographic method was developed. A new RP-18 end-capped column with particle size 2 µm and equilibrated to 35°C in a Shimadzu temperature controller module was used. Four theaflavin monomers were successfully separated in 8 min by the new strategy, comparing to 20–85 min by HPLC in the peer literature reports. Linear gradient elution: from 92% mobile phase A (v) to 76% mobile phase A (v) during early 3 min and then 92% mobile phase A (v) till 8 min at elution flow rate 1.5 ml/min. The limits of detection and quantification were in the range of 0.1–0.3 and 0.4–1.1 mg/l. Satisfactory recoveries of theaflavin, theaflavin-3-gallate, theaflavin-3’-gallate and theaflavin-3,3’-gallate were 97.5–102.6, 98.6–102.4, 99.6–105.4, and 95.5–105.4%, respectively. The new method was applied to quantitative analysis theaflavins of tea samples, including 10 black teas, 5 oolong teas, and 5 green teas. This method is suitable for the rapid, accurate and inexpensive quantitative analysis of theaflavins under the basic detection conditions of HPLC.

Quantitative Analysis of 5-Hydroxymethylfurfural in Linezolid Injection by High Performance Liquid Chromatography

2020 ◽  
Vol 16 (8) ◽  
pp. 1059-1067
Author(s):  
Jéssica Maurício Batista ◽  
Christian Fernandes
Keyword(s):  
High Performance ◽  
Potassium Phosphate ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Official Method ◽  
Ph Variation ◽  
Drug Products ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Background: Linezolid is a synthetic broad-spectrum antibacterial belonging to the class of oxazolidinones. Linezolid for intravenous infusion is isotonized with dextrose. In acidic environment, the dehydration of dextrose produces furan derivatives, 5-hydroxymethylfurfural (5-HMF) being the main one. The determination of this degradation product is of fundamental importance, since there is evidence it is cytotoxic, genotoxic, mutagenic and carcinogenic. However, there is no official method for the determination of 5-HMF in drug products. Objective: The aim of this study was to develop and validate a high performance liquid chromatographic method to quantify 5-HMF in injection of linezolid. Methods: The chromatographic separation, after optimization, was performed on C18 (150 x 4.6 mm, 5 μm) column. Mobile phase was composed of 14 mM potassium phosphate buffer pH 3.0 ([H+] = 1.0 x 10-3) and methanol in gradient elution at 1.0 mL min-1. The injection volume was 10 μL and detection was performed at 285 nm. Results: The method was optimized and validated, showing selectivity, linearity in the range from 0.075 to 9.0 μg mL-1, precision (RSD ≤ 2.0%), accuracy (mean recovery of 100.07%) and robustness for temperature and pH variation. Conclusion: The method was shown to be adequate to determine 5-HMF in injection containing linezolid in routine analysis.

Simultaneous Determination of Six Components in Jingzhiguanxin Tablet by High-Performance Liquid Chromatography

2019 ◽  
Vol 15 (2) ◽  
pp. 130-137
Author(s):  
Hui Jiang ◽  
Lianhao Fu ◽  
Yu Wang ◽  
Shaozhi Wang ◽  
Xiaoxu Zhang ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Gradient Elution ◽  
Tanshinone Iia ◽  
Array Detector ◽  
Control Analysis ◽  
Active Components ◽  
Quality Control Analysis

Background: Jingzhiguanxin (JZGX) tablet, a traditional Chinese prescription, is commonly used for treating coronary heart disease and angina pectoris in the clinic. There are six active components (Danshensu (DSS), Protocatechuic aldehyde (PD), Paeoniflorin (PF), Ferulic acid (FA), Salvianolic acid B (Sal B) and Tanshinone IIA (TA)) in JZGX tablet. </P><P> Objective: In this paper, a simple and reliable method was used for simultaneous determining the six active components by high-performance liquid chromatography coupled with diode array detector (HPLC-DAD). Methods: These six active components were separated on an Agilent Zorbax Eclipse XDB-C18 column (150 mmx4.6 mm, 5 µm) at 30 °C. Acetonitrile (A), methanol (B) and 0.5% H3PO4 aqueous solution (C) were used as mobile phase for gradient elution. The flow rate was 1 mL/min and the detection wavelengths were set at 280 nm for DSS, PD and Sal B, 230 nm for PF, 320 nm for FA and 270 nm for TA, respectively. Results: All of the six components showed good linearity regressions (r2≥0.9997) in the detected concentration range. The recovery rates and coefficient of variation (CV) for all analytes were 98.66%- 100.18% and 0.75%-1.89%, respectively. This method was successfully applied to simultaneously determine the six components in JZGX tablet from different batches and manufacturers. Conclusion: The validated method can be used in routine quality control analysis of JZGX tablet without any interference.

scholarly journals Improved Chromatographic Fingerprinting Combined with Multi-components Quantitative Analysis for Quality Evaluation of Penthorum chinense by UHPLC-DAD

2015 ◽  
Vol 10 (1) ◽  
pp. 1934578X1501000 ◽  
Author(s):  
Wangping Deng ◽  
Tongtong Xu ◽  
Min Yang ◽  
Yajun Cui ◽  
De-an Guo
Keyword(s):  
High Performance ◽  
Herbal Medicines ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Array Detector ◽  
Chromatographic Technique ◽  
Hplc Fingerprint ◽  
Solvent Flow Rate ◽  
Principle Components Analysis ◽  
Penthorum Chinense

A high performance liquid chromatographic (HPLC) fingerprint is commonly used for quality consistency evaluation of herbal medicines. Recently, an improved chromatographic technique resulted in ultra high performance liquid chromatography (UHPLC), which could provide higher resolution in less time under higher pressure using finer particles (less than 2μm) of stationary phase. A simple and sensitive method was developed and validated for fingerprint analysis of Penthorum chinense Pursh (PC), with the simultaneous determination of seven components using UPLC coupled with a diode-array detector (DAD). It took less than 20 min for analysis of one sample. Both similarity analysis and principle components analysis (PCA) were employed to evaluate the quality consistency of 17 sample batches. The analysis was performed on a Waters ACQUITY UPLC HSS T3 (2.1 × 150 mm, 1.7 μm) column, which was maintained at 45°C and the eluents were monitored with DAD at 270 nm. A gradient elution with acetonitrile and water containing 0.075% phosphoric acid was used. The solvent flow rate was 0.4 mL/min. Standard calibration curves showed good linear behavior (R2>0.9994) in the range of 0.20-337.05 μg/mL. Acceptable repeatability (RSD<0.61%), reproducibility (RSD<2.72%), stability (RSD<1.59%) and recovery in the range of 94.7%-102.9% were obtained (precision and accuracy). The validated method was successfully applied to evaluate the quality of 21 samples of PC.

scholarly journals Development and Validation of a Stability-Indicating Column High-Performance Liquid Chromatographic Assay Method for Determination of Nebivolol in Tablet Formulation

2008 ◽  
Vol 91 (3) ◽  
pp. 557-561 ◽  
Author(s):  
Pankaj K Kachhadia ◽  
Ashish S Doshi ◽  
Hitendra S Joshi
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Assay Method ◽  
Array Detector ◽  
Solution Stability ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A simple, precise, and accurate isocratic reversed-phase (RP) stability-indicating column high-performance liquid chromatographic (HPLC) assay method was developed and validated for determination of nebivolol in solid pharmaceutical dosage forms. Isocratic RP-HPLC separation was achieved on a Phenomenex Luna C8 (2) column (250 mm 4.6 mm id, 5 m particle size) using mobile phase composed of acetonitrilepH 3.5 phosphate buffer (35 + 65, v/v) at a flow rate of 1.0 mL/min, and detection was performed at 280 nm using a photodiode array detector. The drug was subjected to oxidation, hydrolysis, photolysis, and heat to apply stress conditions. The method was validated for specificity, linearity, precision, accuracy, robustness, and solution stability. The method was linear in the drug concentration range of 40160 g/mL with a correlation coefficient of 0.9999. The repeatability relative standard deviation (RSD) for 6 samples was 0.69, and the intermediate precision (RSD) for 6 samples was 1.39. The accuracy (recovery) was between 98.57 and 99.55. Degradation products produced as a result of stress studies did not interfere with detection of nebivolol, and the assay can thus be considered stability-indicating.

A High-Performance Liquid Chromatographic Method for the Determination of Meropenem in Serum

2019 ◽  
Vol 58 (2) ◽  
pp. 144-150
Author(s):  
Demet Dincel ◽  
Olcay Sagirli ◽  
Gulacti Topcu
Keyword(s):  
Human Serum ◽  
High Performance ◽  
Chromatographic Method ◽  
Acetic Acid Solution ◽  
High Performance Liquid Chromatographic ◽  
Array Detector ◽  
Therapeutic Drug ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract In this study, a new, sensitive and selective high-performance liquid chromatographic method was developed for the determination of meropenem (MEM) in human serum. In the developed method, C18 column (3.9 × 150 mm, 5 μm) was selected as stationary phase at 30°C, and methanol: acetic acid solution mixture was used as mobile phase with gradient program. Chromatographic separation was carried out at a flow rate of 1 mL/min, and detection was performed at 300 nm with diode array detector. Doripenem was selected as an internal standard, and the analytes were extracted from serum using protein precipitation method with ortho-phosphoric acid: methanol. Detection wavelength was selected as 300 nm. The developed method was validated according to International Council for Harmonisation (ICH) guidelines. The calibration curve was linear over a concentration range of 4–240 μg/mL with correlation coefficient of 0.9985. The limit of detection and limit of quantification values were found as 0.057 and 0.192 μg/mL, respectively. The validated method was successfully applied for the determination of MEM in human serum samples collected from patient volunteers at different time intervals, and therapeutic drug monitoring of MEM has been investigated.

Simultaneous Determination of Seven Active Components in Desheng Pills by High-performance Liquid Chromatography

2020 ◽  
Vol 17 (1) ◽  
pp. 149-158
Author(s):  
Yang Xu ◽  
Huailei Yang ◽  
Baiyu Shan ◽  
Kuo Fang ◽  
Mingyu Li ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
High Performance ◽  
Blood Stasis ◽  
Gradient Elution ◽  
Phosphoric Acid Solution ◽  
Array Detector ◽  
Active Components

Background: Desheng pills (DSP) consist of six traditional Chinese medicine. This preparation is used fornourishing blood, eliminating stasis, soothing liver and regulating menstruation, and can also be used to treat menoxenia and dysmenorrhea caus ed by qi stagnation and blood stasis. Objective: In this paper, an accurate and sensitive high-performance liquid chromatography-diode array detector (HPLC-DAD) method was developed and validated for simultaneous determination of seven active components (gallic acid, paeoniflorin, costunolide, dehydrocostuslactone, rutin, leonurine hydrochloride and ferulic acid) in the traditional Chinese formula-Desheng pills. Methods: The seven analytes were separated on Agilent ZORBAX SB-C18 column (250mm× 4.6mm, 5μm) maintained at the temperature of 30.. Gradient elution was performed with the mobile phase of methanol (A)-0.1% phosphoric acid solution (B) at the flow rate of 1.0mL·min-1. The analysis was carried out at the wavelength of 225 nm, 256 nm, 277 nm and 320 nm with an injection volume of 10 μL. Results: The measured seven components showed good linear relationships within their own concentration ranges along with coefficients of determination ≥0.9996. The limits of detection and quantitation of all analytes were in the range of 0.19-13.51 μg/mL and 0.59-40.93 μg/mL, respectively. Average recoveries ranged from 98.82% to 102.01% with RSDs of 1.47%-1.99%. The content of tested components was in the range of 0.053-0.421 mg/g. Conclusion: The proposed method was found to be sensitive, accurate and reproducible, which provided an effective quantitative analytical method for quality control of Desheng pills.

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