scholarly journals Фенольні сполуки листя Sorbus domestіca і Sorbus graeca

Author(s):  
O. V. Krivoruchko

Introduction. Sorbus domestіca and Sorbus graeca from the Rosaceae family are cultivated in Ukraine in gardens and parks. Their chemical composition is investigated insufficiently.The aim of the study – to research the composition and the content of phenolic compounds of leaves of Sorbus domestіca and Sorbus graeca.Research Methods. The content of phenolic compounds in leaves of Sorbus domestіca and Sorbus graeca was carried out by the high performance liquid chromatography method on Agilent Technologies chromatograph.Results and Discussion. In leaves of Sorbus domestіca chlorogenic acid, rutin, quercetin-3-O-glucoside and quercetin were identified; in leaves of Sorbus graeca chlorogenic and neochlorogenic acids, rutin and 4'-methoxyquercetin-3-O-sophoroside were identified. The content of hydroxycinnamic acids in leaves of Sorbus domestіca is 389 mg/100 g, in leaves of Sorbus graeca – 147 mg/100 g (in terms of chlorogenic acid). The content of flavonoids in leaves of Sorbus domestіca is 1888 mg/100 g, in leaves of Sorbus graeca – 727 mg/100 g (in terms of rutin).Conclusions. The composition and the content of phenolic compounds of Sorbus domestіca and Sorbus graeca were studied by the HPLC method. Leaves of Sorbus domestіca are more perspective for further pharmacological studies.

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (01) ◽  
pp. 35-40
Author(s):  
A. S. Bagde ◽  
V. V. Khanvilkar ◽  

The present work describes a validated reverse phase high performance liquid chromatography (RPHPLC) method for simultaneous estimation of dextromethorphan hydrobromide and quinidine sulphate in pharmaceutical dosage from. The drugs were resolved using Hemochrom Intsil C18-5U column (250×4.6) mm in isocratic mode with mobile phase methanol: water (0.08% diethylamine, 0.02% of glacial acetic acid and pH 4.4 adjusted with orthophosphoric acid) in the ratio of 70:30 V/V at a flow rate of 1.0 mL/min. Retention time of dextromethorphan hydrobromide and quinidine sulphate were 4.9±0.2 and 3.6±0.2, respectively, at 292nm. The above mentioned method was validated as per International Conference on Harmonization (ICH) guidelines. Linear responses were obtained in concentration ranges of 5-35 μg/mL for dextromethorphan hydrobromide and 4-16 μg/mL for quinidine sulphate, with correlation coefficient (r2) of 0.999 for both the drugs. A simple, selective, accurate, precise, robust and reliable RP-HPLC method thus developed and validated for simultaneous estimation of dextromethorphan hydrobromide and quinidine sulphate.


2020 ◽  
Vol 10 (9) ◽  
pp. 1581-1587
Author(s):  
Lei Shi ◽  
Chunqi Liang ◽  
Yongzhi Qi

A sulphurous acid thiolysis-HPLC method for the determination of procyanidins in pine bark products was established. The concentration of sulphurous acid is 1.2%, the concentration of benzyl mercaptan is 2%, the reaction temperature is 90 °C, and the reaction time is 60 minutes. Under these conditions, the preservative rates of catechin, epicatechin, epicatechin gallate and their benzyl sulfide derivatives were 89.7%, 86.2%, 95.4%, 63.1%, 64.6% and 73.5%, respectively. According to this study, the calculation method for the procyanidin content determination by the thiolysis-HPLC method was corrected.


2018 ◽  
Vol 56 (5) ◽  
pp. 803-809 ◽  
Author(s):  
Hannah Rieger ◽  
Patrik Schmidt ◽  
Elke Schaeffeler ◽  
Manabu Abe ◽  
Mira Schiffhauer ◽  
...  

AbstractBackground:Variation in metabolism, toxicity and therapeutic efficacy of thiopurine drugs is largely influenced by genetic polymorphisms in the thiopurine S-methyltransferase (TPMT) gene. Determination of TPMT activity is routinely performed in patients to adjust drug therapy.Methods:We further optimized a previously established high-performance liquid chromatography (HPLC) method by measuring TPMT activity in whole blood instead of isolated erythrocytes, which is based on conversion of 6-mercaptopurine to 6-methylmercaptopurine using S-adenosyl-methionine as methyl donor.Results:The simplified TPMT whole-blood method showed similar or better analytical and diagnostic performance compared with the former erythrocyte assay. The whole-blood method was linear for TPMT activities between 0 and 40 nmol/(mL·h) with a quantification limit of 0.1 nmol/(mL·h). Within-day imprecision and between-day imprecision were ≤5.1% and ≤8.5%, respectively. The optimized method determining TPMT activity in whole blood (y) showed agreement with the former method determining TPMT activity in erythrocytes (x) (n=45, y=1.218+0.882x; p>0.05). Phenotype-genotype concordance (n=300) of the whole-blood method was better when TPMT activity was expressed per volume of whole blood (specificity 92.2%), whereas correction for hematocrit resulted in lower genotype concordance (specificity 86.9%). A new cutoff for the whole-blood method to distinguish normal from reduced TPMT activity was determined at ≤6.7 nmol/(mL·h).Conclusions:This optimized TPMT phenotyping assay from whole blood using 6-MP as substrate is suitable for research and routine clinical analysis.


Author(s):  
B G Keevil ◽  
P W Maylor ◽  
D Rowlands

We developed a binary gradient high-performance liquid chromatography (HPLC) method for measuring HbA2 in whole blood samples using a Pharmacia Mono Q column (1 mL) and measurement at 415 nm. The assay requires a simple lysis and centrifugation step before injection onto the column. We found good agreement of results between the HPLC method and the Helena column chromatography method. The within batch precision was 2·6% and between batch precision was 4·6%. We found that using 30 mM Tris buffers (pH 7·8) with a sodium chloride gradient resulted in short analysis times and good chromatographic separation of HbA2, HbS and HbA. We conclude that this is a robust assay for the diagnosis of β-thalassaemia.


2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Bela Kiss ◽  
Daniela-Saveta Popa ◽  
Marius Bojita ◽  
Felicia Loghin

A high performance liquid chromatography (HPLC) method was developed and validated for determination of flunitrazepam in human plasma. After a simple liquid-liquid extraction, the analyses were carried out on a ODS column with diode array detection at 330nm. The mobile phase consisted in a mixture of potassium dihydrogene phosphate/acetonitrile (40/60, v/v). The method showed good linearity, accuracy and precision. Advantages of this validated assay include a simple plasma extraction method, short analysis time and good sensitivity (LLOQ = 5ng/mL). The stability data indicated a potential instability of flunitrazepam in plasma at room temperature.


2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
Neha Singhal ◽  
Kalpesh Gaur ◽  
Anoop Singh ◽  
Karni Singh Sekhawat

The present study described a new, simple, accurate, and precise high performance liquid chromatography method for the simultaneous determination of Ambroxol and Doxofylline in combined tablet dosage form. The chromatographic method was standardized using a BDS hypersil C18, 250 mm × 4.6 mm, 5 μ (particle size), Thermo scientific from Germany with isocratic conditions, and mobile phase containing potassium dihydrogen orthophosphate buffer-pH 4.5 (0.05 M KH2PO4): acetonitrile (60 : 40) at flow rate of 1 ml/min using UV detection at 254 nm. The retention times of Ambroxol and Doxofylline were 3.510 min and 7.247 min, respectively. The method was linear over the concentration range for Ambroxol 3.75–11.25 μg/mL and for Doxofylline 50-150 μg/mL. The recovery of Ambroxol and Doxofylline was found to be in the range of 99.42–101.18% and 99.37–100.28%, respectively. The validation of method was carried out using ICH guidelines. The described HPLC method was successfully employed for the analysis of pharmaceutical formulations containing combined dosage form.


Author(s):  
MEGHA PATEL ◽  
PARESH PATEL ◽  
DHARA PATEL

Objective: A simple, rapid, accurate, precise, specific, and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) method has been developed and validated for simultaneous estimation of olanzapine (OLZ) and aripiprazole (APR) in synthetic mixtures. Methods: The stationary phase used for chromatographic separation was Phenomenex C18 column (250 mm × 4.6 mm i.d, particle size 5 μm) and mobile phase used for separation was methanol: Phosphate buffer (pH 3) taken in ratio of 75:25 %v/v. The flow rate was used 1.0 ml/min at room temperature and drugs detected at 240 nm with injection volume 20 μL. Results: The retention time for OLZ and APR was found to be 4.231 and 6.523 min, respectively. The linearity was performed using a concentration range of 0.5–3.0 for both drugs. The correlation coefficient was found to be 0.999 for OLZ and APR. The % purity of both the drug was found to be 98–102%. The proposed RP-HPLC method has been validated, according to International council on harmonization Q2 (B) guidelines. Conclusion: There was no interference of any diluents and excipients in the determination of drugs from synthetic mixture. Hence, the developed method can be used for routine quality control analysis.


2019 ◽  
Vol 57 (8) ◽  
pp. 724-729 ◽  
Author(s):  
Mahmoud M Sebaiy ◽  
Wafaa S Hassan ◽  
Mostafa E Elhennawy

Abstract A high performance liquid chromatography method had been developed and validated for rapid simultaneous separation and determination of three anti-helicobacter drugs, oxytetracycline (OXY), tinidazole (TIN) and esomeprazole (ESM) in human plasma within 6 minutes. Drugs extraction method from plasma was based on protein precipitation technique. Separation was carried out on a Equisil BDS C18 column (5 μm, 150 × 4.60 mm) using a mobile phase of acetonitrile: 0.025 M KH2PO4 (25: 75, v/v) adjusted to pH 3.50 with ortho-phosphoric acid at ambient temperature. The flow rate was 1 mL/min and maximum absorption was measured using Diode Array (DAD) detector at 285 nm. The retention times of OXY, TIN and ESM were recorded to be 2.68, 3.52 and 5.17 minutes, respectively, indicating a shorter analysis time. Limits of detection were also reported to be 0.10, 0.07 and 0.04 μg/mL for OXY, TIN and ESM, respectively, showing a high degree of the method sensitivity. The method was then validated according to FDA guidelines for the determination of the drugs clinically in human plasma specially regarding pharmacokinetic and bioequivalence studies.


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