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 Constituents of Da-Cheng-Qi Decoction and its Parent Herbal Medicines Determined by LC-MS/MS

2010 ◽  
Vol 5 (5) ◽  
pp. 1934578X1000500
Author(s):  
Fengguo Xu ◽  
Ying Liu ◽  
Rui Song ◽  
Haijuan Dong ◽  
Zunjian Zhang
Keyword(s):  
High Performance ◽  
Herbal Medicines ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Esi Ms ◽  
Chemical Constitution ◽  
Tandem Mass Spectrometric ◽  
Liquid Chromatographic ◽  
First Time

Da-Cheng-Qi decoction (DCQD) is a purgative prescription used in China and East Asia. To profile the constituents of this complex traditional Chinese medicine (TCM), a high-performance liquid chromatographic, electrospray ionization, tandem mass spectrometric (HPLC-ESI/MS/MS) analytical method was developed. After separation on a reversed-phase C18 analytical column using gradient elution, samples were analyzed by ESI-MS/MS in negative mode. As a result, a total of 37 compounds were detected, of which two tannins, three anthraquinones, two sennosides, five flavonoids and two lignans were unambiguously identified by comparison with standard compounds, and sixteen compounds were either tentatively identified or deduced according to their MS/MS data. The fragmentation pathways of many of the observed compounds, such as the tannins and lignans are reported for the first time. In addition, the identity of each peak in DCQD was explored by comparison with those of its three constituent herbs. The results indicated that tannins, anthraquinones and sennosides in DCQD originated from Radix et Rhizoma Rhei, flavonoids from Fructus Aurantii Immaturus, and lignans from Cortex Magnoliae officinalis. The present study provides an example of chemical constitution profiling in complex TCM systems using LC/MS/MS.

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 Simultaneous Determination of Four Compounds in a Nelumbo nucifera Seed Embryo by HPLC-DAD

2017 ◽  
Vol 2017 ◽  
pp. 1-6 ◽  
Author(s):  
Gahee Ryu ◽  
Jin Bae Weon ◽  
Woo Seung Yang ◽  
Choong Je Ma
Keyword(s):  
High Performance ◽  
Biological Activities ◽  
Herbal Medicines ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Nelumbo Nucifera ◽  
Linear Relationships ◽  
Liquid Chromatographic ◽  
Optimized Conditions

Nelumbo nucifera has a variety of biological activities. So it was importantly used as various herbal medicines since traditional times. A simple, fast, and sensitive high-performance liquid chromatographic (HPLC) method was developed in this study for efficient quality control of N. nucifera. Four different compounds, including neferine, 1,2,3,4-tetrahydro-1-[(4-hydroxyphenyl) methyl]-2-methyl-7-isoquinolinol, 1-hydroxy-2-methylpropene, and 3-(prop-1-enyl)benzene-1,2,4,5-tetrol, were simultaneously determined. The four compounds were isolated through a Dionex C18 column by gradient elution with 0.1% TFA-water and methanol. The flow rate was 1.0 mL/min, and the wavelength was detected at 205, 254, 280, and 330 nm. The chromatograms were acquired at 205 nm. The four compounds showed good linear relationships (r2>0.96) over five different concentrations, and an average recovery of the method ranged from 96.27% to 108.78%. Through the analysis validation test and application of the method, the optimized conditions verified that it is efficient to isolate the compounds of N. nucifera seed embryos.

scholarly journals Development and Validation of a High-Performance Liquid Chromatographic Method for the Simultaneous Quantification of Marker Constituents in Cheonwangbosimdan

2014 ◽  
Vol 9 (12) ◽  
pp. 1934578X1400901
Author(s):  
Chang-Seob Seo ◽  
Hyeun-Kyoo Shin
Keyword(s):  
High Performance ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Array Detector ◽  
Mobile Phases ◽  
Photodiode Array Detector ◽  
Relative Standard ◽  
Development And Validation ◽  
Liquid Chromatographic

A high-performance liquid chromatography–photodiode array detector method was established for the simultaneous determination of 7 components in Cheonwangbosimdan extract. The components were 5-hydroxymethyl-2-furaldehyde (1), coptisine (2), berberine (3), nodakenin (4), harpagoside (5), cinnamic acid (6), and β-asarone (7). All analytes were separated by gradient elution using two mobile phases on a Gemini C18 column and maintained at 40°C. The flow rate was 1.0 mL/min and the injection volume was 10 μL. Calibration curves of the 7 compounds showed good linearity with correlation coefficients ( r2) ≥ 0.9996. The limits of detection and quantification of the 7 analytes were 0.01–0.04 and 0.03–0.12 μg/mL, respectively. The recoveries of the 7 marker constituents were 97.6–104.2% with relative standard deviations (RSD) of less than 2.2%. The RSD values of intra- and interday precision were 0.11–1.78 and 0.19–1.92%, respectively. Among the 7 biomarker compounds, the major compounds of Cheonwangbosimdan were berberine and coptisine, which originated from Coptis japonica. The results indicate that the developed analytical method is suitable for quality control use.

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 HPLC - PDA ANALYSIS OF CAROTENOIDS AND CHLOROPHYLLS FROM CUCURBITA PEPO L.CONVAR.GIROMONTINA FRUITS

1970 ◽  
Vol 62 ◽  
Author(s):  
E. Muntean ◽  
V. Lazăr ◽  
Nicoleta Muntean
Keyword(s):  
High Performance ◽  
Cucurbita Pepo ◽  
Initial Conditions ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Array Detector ◽  
Running Waters ◽  
Photodiode Array Detector ◽  
Photodiode Array

A reversed-phase high-performance liquid chromatographic (HPLC) procedure, which operates with gradient elution and detection by a photodiode-array detector, has been developed to analyze both carotenoids and chlorophylls from the fruits of Cucurbita pepo L.convar.giromontina. HPLC analysis was performed on a system consisting of a 322 Kontron Instruments pumping system, a Rheodyne 7125 injection valve with 20 l loop, a Waters 990 photodiode array detector and a computer running Waters 990 software for data analysis. HPLC separations were achieved on a Nucleosil 120 - 5 C18 column, using the following mobile phases: A - acetonitrile : water (9 : 1) and B - ethyl acetate. The flow rate was 1 ml/ min. and the solvent gradient was as follows: initial conditions - 90% A, 10%B/ from 0 to 15 min. - 30%A, 70% B/ from 16 to 22 min. - 90%A, 10%B. Separations were monitored at 450 nm; peak identities were established by comparing their HPLC retention times and their on-line recorded VIS spectra with those of known reference compounds. Eleven carotenoids were identified: the major ones are -carotene and lutein, these being followed by smaller amounts of neoxanthin, violaxanthin, lactucaxanthin, -cryptoxanthin, -cryptoxanthin, -carotene 5,6-epoxide, -carotene, 9Z--carotene and 15Z--carotene. Besides carotenoids, the proposed procedure separates also chlorophylls a, a’, b, b’, pheophytins a, a’, b and piropheophytins a and b which were identified in unsaponified extracts based on their VIS spectra.

Reversed-Phase High Performance Liquid Chromatographic Analysis of Three First Line Anti-Tuberculosis Drugs

2019 ◽  
Vol 69 (12) ◽  
pp. 3590-3592
Author(s):  
Nela Bibire ◽  
Romeo Iulian Olariu ◽  
Luminita Agoroaei ◽  
Madalina Vieriu ◽  
Alina Diana Panainte ◽  
...  
Keyword(s):  
High Performance ◽  
Biological Fluids ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Assay Method ◽  
Active Pharmaceutical Ingredients ◽  
First Line ◽  
Pharmaceutical Ingredients ◽  
Liquid Chromatographic

Active pharmaceutical ingredients such as isoniazid, pyrazinamide and rifampicin are among the most important first-line anti-tuberculosis drugs. A simple, rapid and sensitive reversed phase-high performance liquid chromatographic assay method for the simultaneous determination of isoniazid, pyrazinamide and rifampicin has been developed. Separation of the interest compounds was achieved in a 10 min chromatographic run in gradient elution mode on a Zorbax SB-C18 stainless steel column (150 � 4 mm, 5 mm) using a guard column containing the same stationary phase. The gradient elution was carried out with a mobile phase of 10% CH3CN aqueous solution for channel A and 50% CH3CN in pH = 6.8 phosphate buffer (20 mM), to which 1.5 mL triethylamine were added for channel B. Quantification of the analyzed substances was carried out spectrophotometrically at 269 nm. Detection limits of 0.48 mg/L for isoniazid, 0.52 mg/L for pyrazinamide and 0.48 mg/L for rifampicin were established for the developed assay method. The present work showed that the proposed analysis method was advantageous for simple and rapid analysis of the active pharmaceutical ingredients in pharmaceuticals and biological fluids.

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.

Supramolecular Solvent Based Liquid-Liquid Microextraction for Preconcentration of Selected Fluoroquinolone Antibiotics in Environmental Water Sample Prior to High Performance Liquid Chromatographic Determination

2019 ◽  
Vol 15 (6) ◽  
pp. 607-615 ◽  
Author(s):  
Shirley K. Selahle ◽  
Philiswa N. Nomngongo
Keyword(s):  
High Performance ◽  
Chromatographic Determination ◽  
Decanoic Acid ◽  
Environmental Water ◽  
High Performance Liquid Chromatographic ◽  
Array Detector ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Supramolecular Solvent ◽  
Liquid Microextraction

Background and Objective: A rapid, simple and environmental friendly supramolecular solvent (SUPRAS) based liquid-liquid microextraction method for preconcentration of ciprofloxacin (CIPRO), danofloxacin (DANO) and enrofloxacin (ENRO) from wastewater was developed. Methods: This microextraction technique was coupled with high-performance liquid chromatography equipped with a diode array detector (HPLC-PDA) for detection and separation of the antibiotics. The SUPRAS composed of decanoic acid and tricaprylymethylammonium chloride. Optimum conditions for the extraction and preconcentration of all the antibiotics were obtained using surface response methodology (RSM) based on Box-Behnken design. Results: Under optimum conditions, the limits of detection (LOD) and limit of quantification (LOQ) ranged from 0.06-0.14 µg L−1 and 0.22-0.47 μg L−1, respectively with the preconcentration factors ranging from 153-241. The linear dynamic ranges were between LOQ and 850 µg L−1 with correlation coefficients ranging from 0.9928 to 0.9999. The intra-day (n = 15) and inter-day (n = 5) precisions (expressed in terms of %RSD) for 50 µg L−1 of CIPRO, DANO and ENRO were in the range of 3.3–4% and 4.1–5.8%, respectively. Conclusion: Lastly, the developed method was used for the extraction, preconcentration and quantification of selected CIPRO, DANO and ENRO in influent and effluent wastewater samples.

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