scholarly journals MÉTODO DE VALIDAÇÃO E SEPARAÇÃO DE ISOFLAVONAS PRESENTES EM MELAÇO DE SOJA

e-xacta ◽  
2018 ◽  
Vol 11 (1) ◽  
pp. 97
Author(s):  
Daniel Mantovani ◽  
Aline Takaoka Alves Baptista ◽  
Charleston De Oliveira Bezerra ◽  
Driano Rezende ◽  
Luis Fernando Cusioli ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Human Body ◽  
Hplc Analysis ◽  
High Efficiency ◽  
Limit Of Detection ◽  
The Body ◽  
Physiological Effects ◽  
Analysis Method ◽  
Limit Of Quantification ◽  
Functional Forms

<p><em>As isoflavonas atuam no organismo humano com efeitos fisiológicos de forma benéfica tornando os alimentos que contém isoflavonas em formas funcionais ao organismo. Assim, neste trabalho foi desenvolvido um método de análise por Cromatografia Líquida de Alta Eficiência (CLAE) bem como, separação e quantificação de isoflavonas presentes no melaço de soja. A validação do método foi baseada pela linearidade, limite de detecção (LD) e limite de quantificação (LQ) com estabelecimentos de critérios de análise para aceitação da metodologia proposta. Os resultados obtidos na separação dos isômeros de isoflavonas bem como a quantificação trouxeram melhorias relacionadas ao tempo de retenção de cada isômero estudado e separação dos compostos. Com relação ao método aplicado ao longo do estudo este apresentou resultados pertinentes para utilização e expansão do método proposto focado nos compostos de isoflavonas formas glicosídicas e agliconas presentes no melaço de soja.</em></p><p> </p><p><em>ABSTRACT</em></p><p><em>Isoflavones act in the human body with physiological effects in a beneficial way making foods containing isoflavones in functional forms to the body. Thus, in this work a high efficiency liquid chromatography (HPLC) analysis method was developed, as well as, separation and quantification of isoflavones from in soybean molasses. The validation of the method was based on linearity, limit of detection (LD) and limit of quantification (LQ) with establishments of analysis criteria for acceptance of the proposed methodology. The results obtained in the separation of the isoflavone isomers as well as the quantification brought improvements related to the retention time of each studied isomer and separation of the compounds. In relation to the method applied throughout the study, it presented relevant results for the use and expansion of the proposed method focused on the isoflavone compounds glycosidic forms and aglycones from soybean molasses.</em></p>

scholarly journals Simultaneous Quantification of Eight Marker Components in Traditional Herbal Formula, Haepyoyijin-Tang Using HPLC–PDA

2020 ◽  
Vol 10 (11) ◽  
pp. 3888
Author(s):  
Chang-Seob Seo ◽  
Mee-Young Lee
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Analysis Method ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Mulberroside A ◽  
Quantitative Analyses ◽  
Main Components ◽  
Herbal Prescription

Haepyoyijin-tang (HPYJT) is a traditional herbal prescription that is composed of 12 medicinal herbs. Although HPYJT is frequently used in patients with asthma in Korea, no quality assessment protocols have been developed. In the present study, qualitative and quantitative analyses were performed using high-performance liquid chromatography and liquid chromatography–tandem mass spectrometry on the eight main components (mulberroside A, amygalin, liquiritin apioside, liquiritin, narirutin, hesperidin, rosmarinic acid, and glycyrrhizinic acid) to establish a quality control protocol for HPYJT. The simultaneous analysis method developed was satisfactorily validated with respect to linearity, limit of detection, limit of quantification, recovery, and precision. This analytical method thus provides an efficient approach for the evaluation of HPYJT quality.

scholarly journals Quantification of plasma remdesivir and its metabolite GS-441524 using liquid chromatography coupled to tandem mass spectrometry. Application to a Covid-19 treated patient

2020 ◽  
Vol 58 (9) ◽  
pp. 1461-1468 ◽  
Author(s):  
Jean-Claude Alvarez ◽  
Pierre Moine ◽  
Isabelle Etting ◽  
Djillali Annane ◽  
Islam Amine Larabi
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Half Life ◽  
Limit Of Detection ◽  
Treated Patient ◽  
Internal Standard ◽  
Therapeutic Drug ◽  
Active Metabolites ◽  
Limit Of Quantification ◽  
Positive Mode

AbstractObjectivesA method based on liquid chromatography coupled to triple quadrupole mass spectrometry detection using 50 µL of plasma was developed and fully validated for quantification of remdesivir and its active metabolites GS-441524.MethodsA simple protein precipitation was carried out using 75 µL of methanol containing the internal standard (IS) remdesivir-13C6 and 5 µL ZnSO4 1 M. After separation on Kinetex® 2.6 µm Polar C18 100A LC column (100 × 2.1 mm i.d.), both compounds were detected by a mass spectrometer with electrospray ionization in positive mode. The ion transitions used were m/z 603.3 → m/z 200.0 and m/z 229.0 for remdesivir, m/z 292.2 → m/z 173.1 and m/z 147.1 for GS-441524 and m/z 609.3 → m/z 206.0 for remdesivir-13C6.ResultsCalibration curves were linear in the 1–5000 μg/L range for remdesivir and 5–2500 for GS-441524, with limit of detection set at 0.5 and 2 μg/L and limit of quantification at 1 and 5 μg/L, respectively. Precisions evaluated at 2.5, 400 and 4000 μg/L for remdesivir and 12.5, 125, 2000 μg/L for GS-441524 were lower than 14.7% and accuracy was in the [89.6–110.2%] range. A slight matrix effect was observed, compensated by IS. Higher stability of remdesivir and metabolite was observed on NaF-plasma. After 200 mg IV single administration, remdesivir concentration decrease rapidly with a half-life less than 1 h while GS-441524 appeared rapidly and decreased slowly until H24 with a half-life around 12 h.ConclusionsThis method would be useful for therapeutic drug monitoring of these compounds in Covid-19 pandemic.

High performance liquid chromatography (HPLC) method development and validation for the determination of flunixin: Animal plasma based study

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Mobile Phases ◽  
Hplc Method Development ◽  
Development And Validation

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.

scholarly journals Oxytetracycline Residues in Honey Analyzed by Liquid Chromatography with UV Detection

2013 ◽  
Vol 57 (1) ◽  
pp. 25-32 ◽  
Author(s):  
Anna Gajda ◽  
Andrzej Posyniak ◽  
Andrzej Bober ◽  
Tomasz Błądek ◽  
Jan Żmudzki
Keyword(s):  
Liquid Chromatography ◽  
Oxalic Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Experimental Treatment ◽  
Uv Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method

Summary A liquid chromatography method with UV detection for determination of oxytetracycline (OTC) in honey has been developed. The samples were extracted with the solution of oxalic acid. The clean-up procedure was performed by solid phase extraction (SPE) using polymeric Strata X and carboxylic acid cartridges. Chromatographic separation was carried out on the Luna C8 analytical column with mobile phase consisting of acetonitrile-0.02 M oxalic acid. The method has been successfully validated according to the requirements of the European Decision 2002/657/EC and this method is used in routine control of oxytetracycline in honey samples. The limit of detection (LOD) and limit of quantification (LOQ) of the presented method were 10 and 12.5 μg/kg, respectively. The developed method has also been verified in quantitative determination of oxytetracycline residues in honey after experimental treatment with this product in bee colonies.

scholarly journals LC-MS characterization of acid degradation products of metoclopramide: Development and validation of a stability-indicating RP-HPLC method

2020 ◽  
Vol 11 (1) ◽  
pp. 781-789
Author(s):  
Sriram Valavala ◽  
Nareshvarma Seelam ◽  
Subbaiah Tondepu ◽  
Suresh Kandagatla
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Hplc Technique

The present study aims to develop a simple, accurate and specific stability-indicating RP-HPLC technique for the analysis of metoclopramide in the presence of its stress degradation products and characterization of degradation compounds by LC-MS/MS analysis. As per ICH Q1A-R2 guidelines, the drug was exposed to acid hydrolytic stress condition. Three degradation products were formed for MCP in acid hydrolysis. The liquid chromatography was processed on a Luna C18-(2) 100A,250×4.6mm 5micron column using an isocratic mobile phase consisting of 0.1% formic acid in water-acetonitrile (20:80, v/v) by adjusting the mobile phase at 1 ml/min flow rate with wavelength detection at 273 nm. The developed procedure was applied to LC-MS/MS (liquid chromatography-tandem mass spectrometry) for the characterization of all the degradant components. Total new three degradation compounds were recognized and identified by LC-MS/MS. The developed RP-HPLC technique was validated as per the ICH Q2-R1 guidelines. Limit of detection and limit of quantification values of MCP were evaluated from the linearity graph and were found to be 5.23 µg/ml and 17.44 µg/ml. Accuracy study was established at 80.0, 100.0 and 120.0 µg/ml concentration levels and the findings were found in the range of 98.4% - 101.8%. The linearity of the technique was assessed over the drug concentration range of 50.0 µg/ml to 250.0 µg/ml and the regression equation, slope and correlation coefficient values were found to be y = 10618x + 1623.2, 10618 and 0.9996 respectively. The developed technique was uninterruptedly applied for the quantification of metoclopramide inactive pharmaceuticals.

scholarly journals ESTIMATION OF GUGGULSTERONE-Z IN GOKSHURADI GUGGULU USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2018 ◽  
Vol 11 (11) ◽  
pp. 204
Author(s):  
Kanan G Gamit ◽  
Niraj Y Vyas ◽  
Nishit D Patel ◽  
Manan A Raval
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Photodiode Array Detector ◽  
Validation Parameters ◽  
Photodiode Array

Objective: A study was aimed to estimate guggulsterone-Z (GZ) in Gokshuradi Guggulu (GG).Methods: An analytical method was developed and validated using Waters Alliance high-performance liquid chromatography system (Empower software), equipped with photodiode array detector. Separation was achieved using Phenomenex, C-18 (250 mm×4.6 mm, 5 μ) column. Mobile phase consisted of acetonitrile:water (70:30,v/v). Flow rate was set to 1 ml/min and detection was performed at 251 nm.Results and Discussion: Validation parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, and robustness were performed. Amount of GZ was estimated using linearity equation.Conclusion: GG was found to contain 0.815±0.03 g% w/w GZ. Validated method may be used as one of the parameters to standardize the formulation.

scholarly journals Estimation of Abamectin Residues Present in Tea: High-Performance Liquid Chromatography Technique

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Madasamy Kottiappan ◽  
Shanmugaselvan Veilumuthu Anandhan ◽  
Selvaganapathi Chandran
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Black Tea ◽  
Water Mixture ◽  
Fluorescence Detector ◽  
Limit Of Quantification ◽  
Acetone Water ◽  
Sensitive Method

A simple, reliable, and sensitive method was based on high-performance liquid chromatography (HPLC) was developed and validated for the estimation of abamectin residues present in tea. The abamectin residues extracted with acetone-water mixture (70 : 30, v/v) and derivatised with 1-methylimidazole (1-MIM) and trifluoroacetic anhydride (TFAA) were estimated by HPLC using fluorescence detector (FLD). The technique was validated in terms of linearity, precision, recovery, specificity, limit of detection (LOD), and limit of quantification (LOQ). A good linear relationship () was absorbed in the abamectin concentration range from 0.01 to 1.0 μg mL−1. The limit of detection and limit of quantification of the method were 0.01 and 0.02 μg g−1, respectively. The average recoveries of the pesticide from black tea and dried green leaves ranged from 83.3 to 103.8% and 83.8 to 98.0%, respectively.

The Application of the Human Body Link Stress Analysis Method in the Basketball Movement

2017 ◽  
Vol 14 (1) ◽  
pp. 79-83
Author(s):  
Man Wang
Keyword(s):  
Stress Analysis ◽  
Human Body ◽  
Teaching Practice ◽  
The Body ◽  
Analysis Method ◽  
Body Movements ◽  
And Training ◽  
Original Dynamic

“Link stress analysis method” is a method to determine to cause the original dynamic muscle of the body movements. In the basketball sports and training, it gets more and more attention. The writer tries to base the teaching practice, to make some supplement and discussion of the theoretical definition, the methods of the analysis of the original muscle and the problems that should be noticed.

scholarly journals Presence of zearalenone in the most commonly grown wheat cultivars in Serbia

2013 ◽  
pp. 101-109 ◽  
Author(s):  
Igor Jajic ◽  
Sasa Krstovic ◽  
Biljana Perisic ◽  
Sandra Jaksic ◽  
Vojislava Bursic ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Phase Extraction ◽  
Wheat Cultivars ◽  
Limit Of Quantification ◽  
Average Value ◽  
Contamination Levels ◽  
Maximum Limit

A total of 45 samples of wheat from three different locations in Vojvodina were analyzed for the presence of zearalenone. Analytical methods based on clean-up by solid-phase extraction (SPE) columns and detection by liquid chromatography were used after validation. Limit of detection for ZEA in wheat was 18.6 ?g/kg and the limit of quantification was 56.5 ?g/kg. Recovery values ranged between 86% and 97%. The occurrence of ZEA in wheat was rather high with 53.3% of positive samples with the average value of 330 ?g/kg. Incidences were found from 68 ?g/kg to 1079 ?g/kg. Contamination levels were above the established maximum limit for unprocessed cereals, other than maize, in as many as seventeen samples. These results were compared to the results of investigation of deoxynivalenol and fumonisin content, established in our previous work on the same samples. The results obtained were also compared to those of the neighboring countries where the relevant data existed and to the data of previous studies in our country.

scholarly journals Rapid Screening and Quantitative Determination of Active Components in Qing-Hua-Yu-Re-Formula Using UHPLC-Q-TOF/MS and HPLC-UV

2018 ◽  
Vol 2018 ◽  
pp. 1-11 ◽  
Author(s):  
Xin Shao ◽  
Jie Zhao ◽  
Xu Wang ◽  
Yi Tao
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Chemical Constituents ◽  
Rapid Screening ◽  
Active Components ◽  
Limit Of Quantification ◽  
Unknown Compound ◽  
Salvianolic Acid ◽  
Tof Ms

Qing-Hua-Yu-Re-Formula (QHYRF), a new herbal preparation, has been extensively used for treating diabetic cardiomyopathy. However, the chemical constituents of QHYRF remain uninvestigated. In the present study, rapid ultrahigh-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UHPLC-Q-TOF/MS) was used to qualitatively analyze the components of QHYRF. Qualitative detection was performed on a Kromasil C18 column through the gradient elution mode, using acetonitrile-water containing 0.1% formic acid. Twenty-seven compounds were identified or tentatively characterized, including 12 phenolic acids, nine monoterpene glycosides, two flavonoids, three iridoids, and one unknown compound. Among these, six compounds were confirmed by comparing with standards. A high-performance liquid chromatography (HPLC) method was developed to simultaneously determine the following six active components in QHYRF: danshensu, paeoniflorin, acteoside, lithospermic acid, salvianolic acid B, and salvianolic acid C. These HPLC chromatograms were monitored at 254, 280, and 320 nm. The method was well validated with respect to specificity, linearity, limit of detection, limit of quantification, precision, stability, and recovery. The HPLC-UV method was successfully applied to 10 batches of QHYRF.

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