scholarly journals Simultaneous Determination of Contents of Flavonol Glycosides and Terpene Lactones in Ginkgo Biloba Tablets by Ultra High Performance Liquid Chromatography Tandem Single Quadrupole Mass Spectrometry Detector

2020 ◽  
Author(s):  
Lin Ma ◽  
Jie Zhang ◽  
Wei-rong Jin ◽  
Siwang Wang
Keyword(s):  
Ginkgo Biloba ◽  
Recovery Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Cerebrovascular Diseases ◽  
Mass Spectrometry Detector ◽  
Good Repeatability ◽  
Sample Recovery

AbstractGinkgo biloba leaf tablets is an effective ingredient in the treatment of cardiovascular and cerebrovascular diseases. In the process of drug production, the quality of ginkgo preparations is often controlled by measuring the content of seven ingredients in ginkgo leaves. To establish UPLC-MS multicomponent analysis method for ginkgo biloba tablets and to simultaneously determine the contents of quercetin (QUE), isorhamnetin(ISO), kaempferol(KAE) and GinkgolideA (GA),ginkgolideB(GB),ginkgolideC(GC) and bilobalide (BB) in ginkgo tablets. Waters Xbridge C18(4.6×150mm,3.5um) column was used, mobile phase A was acetonitrile and mobile phase B was water (containing 0.10% formic acid). The injection volume was 10μL.Negative ion mode monitoring was conducted with ESI. Scanning range:m/z100∼1400.The detection ions of the seven tested components includem/z301.0(QUE),m/z284.9(KAE),m/z315.1(ISO),m/z453.1(GA),m/z423.1(G B),m/z439.0(GC)and m/z325.0(BB), respectively. Within a space of 10min, flavonoids and terpene lactones in ginkgo biloba tablets were completely separated. The peak area exhibited an excellent linear relationship with the concentration. The sample recovery rate ranged from 91.74% to 109.77%.Precision RSDs of within-day and between-day were lower than 2.879% and 3.928% respectively. The method for determination of seven components in ginkgo biloba tablets displays good repeatability, recovery rate and precision, for which it can be applied to quality control of ginkgo biloba tablets.

scholarly journals Development and Validation of a HPLC-UV Method with Pre-column Derivatization for Determination of Cinnabar in Jufang Zhibao Pills

2017 ◽  
Vol 5 (02) ◽  
pp. 01-09
Author(s):  
Xin Zhang ◽  
Jia Yao ◽  
Ying Ren ◽  
Yuan Li ◽  
Zhimin Xie
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
High Accuracy ◽  
Chromatography Method ◽  
Average Recovery ◽  
Sem Image ◽  
Good Repeatability ◽  
Liquid Chromatography Method ◽  
Development And Validation

In this work, a reliable and accurate high-performance liquid chromatography method with pre-column derivatization was established and validated for determination of cinnabar in Jufang Zhibao pills. Scanning electron microscope (SEM) image was used to identify the types of cinnabar crude drug in Jufang Zhibao pills. The chromatography separation was performed on a Welch XB-C18 column (250 mm × 4.6 mm, 5 μm). The mobile phase consists of water spiked with 0.022 mmol/L sodium diethyldithiocarbamate (A, pH adjusted to 8–9 by ammonia water) and methanol (B, 80:20, v/v) at flow rate of 1.0 ml/min with the detected wavelength was 272 nm. The oven temperature was set at 35°C. The calibration for cinnabar content has good linearity (R2 =0.9999) over the range of 2.43–300 μg/ml and the average recovery was less then 1.90%. The limits of detection and quantification were 0.1127 μg and 0.2065 μg/ml. The results indicated that the proposed method has advantages of high accuracy, good repeatability and stability and can be successfully used for determination of cinnabar in Jufang Zhibao pills. It provides a basis for drug manufacture quality control and proves the feasibility of the pre-column derivatization method during the determination of cinnabar in Jufang Zhibao pills.

scholarly journals Determination of Carbamazepine and Its Impurities Iminostilbene and Iminodibenzyl in Solid Dosage Form by Column High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (4) ◽  
pp. 1059-1068 ◽  
Author(s):  
Predrag Lj Džodić ◽  
Ljiljana J ivanovi ◽  
Ana D Proti ◽  
Mira L Zeevi ◽  
Biljana M Joci
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Solid Dosage ◽  
Rp Hplc ◽  
Good Repeatability ◽  
Chemometric Approach

Abstract An accurate and precise RP-HPLC method was developed and validated for the determination of carbamazepine and its impurities iminostilbene and iminodibenzyl in a tablet formulation with fluphenazine as an internal standard. Buffermethanol (50 + 50, v/v) was used as the mobile phase. During validation, specificity, linearity, precision, accuracy, LOD, LOQ, and robustness of the method were tested. The method was proven to be specific against placebo interference. Linearity was evaluated over the concentration range of 100500, 0.050.25, and 0.10.5 g/mL, and the r values were 0.9994, 0.9997, and 0.9979 for carbamazepine, iminostilbene, and iminodibenzyl, respectively. Intraday precision of the method was good, and RSD was below 2 for all analytes. The accuracy of the method ranged from 100.69 to 102.10, 99.76 to 102.66, and 99.26 to 100.08 for carbamazepine, iminostilbene, and iminodibenzyl, respectively. LOD was 0.0125, 0.025, and 0.05 g/mL and LOQ was 0.05, 0.05, and 0.1 g/mL for carbamazepine, iminostilbene, and iminodibenzyl, respectively. Robustness of the method was proven by using a chemometric approach. The method was successfully applied to the analysis of commercially available carbamazepine tablets and showed good repeatability, with RSD below 2.

scholarly journals Determination of eight lignans in Schisandra chinensis and Schisandra sphenanthera

2016 ◽  
Vol 11 ◽  
pp. S161-S167 ◽  
Author(s):  
Xu Guangyu ◽  
Niu Jiamu ◽  
Yuan Guangxin ◽  
Bai Yu ◽  
Li Hongyu ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Gradient Elution ◽  
Schisandra Chinensis ◽  
Chromatography Method ◽  
Schisandra Sphenanthera ◽  
Content Determination ◽  
Liquid Chromatography Method

A high performance liquid chromatography method for the determination of eight lignans contents in Schisandra chinensis and Schisandra sphenanthera was developed. The chromatographic column was Agilent ZORBAX 300SB-C18 column (4.6 mm × 250 mm?5 ?m). The mobile phase was methanol-water, a gradient elution was conducted and the detection wavelength was at 230 nm. The results showed that the recovery rate of eight lignans was 92.2-102.9% and RSD was 1.5-4.2%. The established content determination method was simple, sensitive, accurate and stable, and can be used to control the quality of S. chinensis and S. sphenanthera. 

scholarly journals A Study on the Determination of Azithromycin by High-Performance Liquid Chromatography

2021 ◽  
Vol 5 (4) ◽  
pp. 125-130
Author(s):  
Yanli Zhuo
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Recovery Rate ◽  
High Performance ◽  
Drug Content ◽  
External Standard Method ◽  
Relative Standard ◽  
Theoretical Plate Number ◽  
Good Repeatability

Objective: To analyze the effect of high-performance liquid chromatography (HPLC) for the determination of azithromycin and to provide references for related research work. Methods: The mobile phase was ammonium dihydrogen phosphate at 0.067 mol/L (mixed with triethylamine; pH value was adjusted to 6.5). The chromatographic column was Kromasil C18 (250 mm × 4.6 mm; 5.0 ?m) and the relative standard deviation (RSD) of the drug content level was 1.25%. The injection volume was set to 20 ?L, the detection wavelength was set to 210 nm, the external standard method was used to complete the quantitative work, and the theoretical plate number should be more than 1000 according to the drug peak calculation. The effect of HPLC on the determination of azithromycin was analyzed. Results: The concentration of azithromycin was 1.40-3.40 mg/mL, and the linear relationship was good. RSD of the drug content level was 1.25%. The representative test product had strong stability within 8.0 hours and the method had good repeatability. According to the recovery experiment method, the recovery rates of three standard samples from low to high were 99.87%, 100.15%, and 100.62%. The average recovery rate was 100.21%. RSD value was 0.39%. It means that the recovery rate of HPLC is good. Conclusion: In the determination of azithromycin, the use of HPLC to complete the work was of high sensitivity, simple, and fast. The method had good repeatability in the determination of drug components which is worthy of further promotion.

Contribution to the Optimization of a Gas Chromatographic Method by QbD Approach used for Analysis of Essential Oils from Salvia officinalis

2019 ◽  
Vol 70 (6) ◽  
pp. 2015-2020
Author(s):  
Silvia Robu ◽  
Aurelia Romila ◽  
Olimpia Dumitriu Buzia ◽  
Adrian Florin Spac ◽  
Camelia Diaconu ◽  
...  
Keyword(s):  
Essential Oil ◽  
Essential Oils ◽  
Plant Material ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Salvia Officinalis ◽  
Salvia Officinalis L ◽  
Gas Chromatographic Method

Numerous articles on Salvia officinalis L. have been published regarding the composition of their essential oil. The considerable variation found may be due to the quality of the plant material as well as to the methods used for analysis. A simple GC-MS method was developed and optimized in the QbD approach, for the determination of sage essential oils. The optimization of GC-MS analysis was performed using different mobile phase flows, injection volumes, split ratios and temperature programs. The optimized method proved to be simple and can be successfully applied for the determination of sage essential oils.

The Dtermination of Paracetamol by HPLC Validation of the Method and Application on Serum Samples

2018 ◽  
Vol 69 (3) ◽  
pp. 627-631 ◽  
Author(s):  
Viorica Ohriac (Popa) ◽  
Diana Cimpoesu ◽  
Adrian Florin Spac ◽  
Paul Nedelea ◽  
Voichita Lazureanu ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Hplc Analysis ◽  
Emotional Experience ◽  
Optimum Conditions ◽  
Serum Samples ◽  
Liquid Chromatograph ◽  
Mobile Phase Flow Rate ◽  
Quantification Limit

Pain is defined as a disagreeable sensory and emotional experience related to a tissue or potential lesion. Paracetamol (Acetaminophen) is the most used non-morphine analgesic. For the determination of paracetamol we developed and validated the high performance liquid chromatography (HPLC) analysis using a Dionex Ultimate 3000 liquid chromatograph equipped with a multidimensional detector. After determining the optimum conditions of analysis (80/20 water / acetonitrile mobile phase, flow rate 1.0 mL / min, detection wavelength 245 nm) we validated the method following the following parameters: linearity of response function, linearity of results, limit (LD = 0.66 mg / mL) and quantification limit (LQ = 2.00 mg / mL), and precision. The method of determining paracetamol by HPLC was applied to 30 samples of serum collected from patients who had pain and were treated with paracetamol.

Optimum HPLC Conditions for Determination of Dibucaine HCL, Fluocortolone Pivalate and Fluocortolone Caproate by Using Experimental Design

2018 ◽  
Vol 15 (1) ◽  
pp. 32-38 ◽  
Author(s):  
Bürge Aşçı ◽  
Mesut Koç
Keyword(s):  
Experimental Design ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Acid Mixture ◽  
Solution Stability ◽  
Uv Detector

Introduction:This paper presents the development and validation of a novel, fast, sensitive and accurate high performance liquid chromatography (HPLC) method for the simultaneous quantitative determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical preparations.Experiment:Development of the chromatographic method was based on an experimental design approach. A five-level-three-factor central composite design requiring 20 experiments in this optimization study was performed in order to evaluate the effects of three independent variances including mobile phase ratio, flow rate and amount of acid in the mobile phase.Conclusion:The optimum composition for mobile phase was found as a methanol:water:acetic acid mixture at 71.6 : 26.4 : 2 (v/v/v) ratio and optimum separation was acquired by isocratic elution with a flow rate of 1.3 mL/min. The analytes were detected using a UV detector at 240 nm. The developed method was validated in terms of linearity, precision, accuracy, limit of detection/quantitation and solution stability and successfully applied to the determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical topical formulations such as suppositories and ointments.

Separation and Determination of Some Aromatic Sulfones by Reversed-Phase High-Performance Liquid Chromatography

1994 ◽  
Vol 59 (3) ◽  
pp. 569-574 ◽  
Author(s):  
Josef Královský ◽  
Marta Kalhousová ◽  
Petr Šlosar
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Uv Spectra ◽  
Optimum Conditions ◽  
Linear Calibration ◽  
Technical Grade

The reversed-phase high-performance liquid chromatography of some selected, industrially important aromatic sulfones has been investigated. The chromatographic behaviour of three groups of aromatic sulfones has been studied. The optimum conditions of separation and UV spectra of the sulfones and some of their hydroxy and benzyloxy derivatives are presented. The dependences of capacity factors vs methanol content in mobile phase are mentioned. The results obtained have been applied to the quantitative analysis of different technical-grade samples and isomer mixtures. For all the separation methods mentioned the concentration ranges of linear calibration curves have been determined.

scholarly journals Simultaneous Determination of Preservatives (Methyl Paraben and Propyl Paraben) in Sucralfate Suspension Using High Performance Liquid Chromatography

2011 ◽  
Vol 8 (1) ◽  
pp. 340-346 ◽  
Author(s):  
Rajesh M. Kashid ◽  
Santosh G. Singh ◽  
Shrawan Singh
Keyword(s):  
High Performance Liquid Chromatography ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Reversed Phase Hplc ◽  
Methyl Paraben ◽  
Propyl Paraben

A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P.) and propyl paraben (P.P.) is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50) on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precision, specificity, linear range and reproducibility were evaluated. The developed method was applied for the determination of preservative M.P. and P.P. at concentration of 0.01 mg/mL and 0.1 mg/mL respectively. The method was successfully used for determining both compounds in sucralfate suspension.

Determination of adenine nucleotides by the modified method of high-performance liquid chromatography

2021 ◽  
Vol 66 (3) ◽  
pp. 172-176
Author(s):  
Lyubov Borisovna Kalikova ◽  
E. R. Boyko
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Adenine Nucleotides ◽  
Release Time ◽  
Chromatography Method ◽  
Rp Hplc ◽  
Standard Solutions

Adenine nucleotides (ATP, ADP and AMP) play a central role in the regulation of metabolism and energy: they provide the energy balance of the cell, determine its redox state, act as allosteric effectors of a number of enzymes, modulate signaling and transcription factors and activate oxidation or biosynthesis substrates. A large number of methods have been developed to determine the level of ATP, ADP and AMP, but the most universal and effective method for the separation and analysis of complex mixtures is the reversed-phase high-performance liquid chromatography method (RP-HPLC). The aim of this study is to determine the optimal conditions for the qualitative separation and quantitative determination of standard solutions of ATP (1 mmol/l), ADP (0,5 mmol/l) and AMP (0,1 mmol/l) by RP-HPLC. The degree of separation of adenine nucleotides was estimated by the time of peak output in the chromatogram. To achieve the goal, the following tasks were set: assess the effect of the temperature of the analysis on the separation and change of the release time of the analytes in the chromatogram; determine the most optimal composition of the mobile phase for the separation of ATP, ADP and AMP in the chromatogram (the content of the organic solvent in the solution); to identify the effect of pH of the mobile phase on the separation of standard solutions of adenine nucleotides; set the optimal molarity of the mobile phase for the separation of ATP, ADP and AMP in the chromatogram. It was found that the temperature of the analysis does not affect the quality of peak separation, while the composition and pH of the mobile phase have a significant effect on the complete and clear separation of the studied nucleotides in the chromatogram. It was determined that the analysis temperature of 37°C and the mobile phase of 0.05 M KH2PO4 (pH 6.0) are optimal for separating the peaks of adenine nucleotides.

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