scholarly journals Development and Validation of Sibutramine Determination in Drug Products by Capillary Electrophoresis

2020 ◽  
Vol 9 (4) ◽  
pp. 141-145
Author(s):  
A. M. Sukhanova ◽  
I. B. Perova ◽  
K. I. Eller ◽  
G. M. Rodioinova ◽  
S. V. Chernova ◽  
...  
Keyword(s):  
Capillary Electrophoresis ◽  
Quantitative Determination ◽  
Limit Of Detection ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Limit Of Quantification ◽  
Drug Products ◽  
Development And Validation

Introduction. Recently, there has been a growing trend in the number of obese and overweight patients. To date, sibutramine is the most effective drug for treating obesity and overweight. The drug is an inhibitor of the reuptake of serotonin and norepinephrine, which leads to a decrease in hunger, and therefore, to weight loss.Aim. To develop and validate a methodology for the determination of sibutramine in drugs by capillary electrophoresis (CE) using an ultraviolet diode array detector.Materials and methods. Quantitative determination of sibutramine in drugs was carried out using the CE method with an ultraviolet diode array detector. A solution of phosphate buffer 50 mmol pH = 7.0 was used as a solvent and working electrolyte; to separate the peaks – quartz capillary 56 cm, 50 μm.Results and discussion. The developed method was validated according to the following parameters: specificity, linearity, correctness, precision, limit of detection and limit of quantification.Conclusion. A method for the quantitative determination of sibutramine in drugs by the CE method using an ultraviolet diode array detector has been developed and validated. This method meets all the requirements of General Pharmacopoeia Monograph 1.1.0012.15 «Validation of the analytical method» and can be used to control the quality of drugs, the active pharmaceutical substance of which is sibutramine.

Screening method for the determination of tetracyclines and fluoroquinolones in animal drinking water by liquid chromatography with diode array detector

2015 ◽  
Vol 18 (2) ◽  
pp. 283-289 ◽  
Author(s):  
E. Patyra ◽  
E. Kowalczyk ◽  
A. Grelik ◽  
M. Przeniosło-Siwczyńska ◽  
K. Kwiatek
Keyword(s):  
Drinking Water ◽  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Screening Method ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Limit Of Quantification

Abstract A liquid chromatography – diode array detector (HPLC-DAD) procedure has been developed for the determination of oxytetracycline (OTC), tetracycline (TC), chlorotetracycline (CTC), doxycycline (DC), enrofloxacin (ENR), ciprofloxacin (CIP), sarafloxacin (SAR) and flumequine (FLU) residues in animal drinking water. This method was applied to animal drinking water. Solid-phase extraction (SPE) clean-up on an Oasis HLB cartridge allowed an extract suitable for liquid chromatographic analysis to be obtained. Chromatographic separation was carried out on a C18 analytical column, using gradient elution with 0.1% trifluoroacetic acid – acetonitrile – methanol at 30°C. The flow-rate was 0.7 mL/min and the eluate was analysed at 330 nm. The whole procedure was evaluated according to the requirements of the Commission Decision 2002/657/EC, determining specificity, decision limit (CCα), detection capacity (CCβ), limit of detection (LOD), limit of quantification (LOQ), precision and accuracy during validation of the method. The recoveries of TCs and FQs from spiked samples at the levels of 10, 100 and 1000 μg/L were higher than 82%. The developed method based on HPLC-DAD has been applied for the determination of four tetracyclines and four fluoroquinolones in animal drinking water samples.

scholarly journals DEVELOPMENT AND VALIDATION OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY WITH DIODE ARRAY DETECTOR METHOD TO ANALYSIS OF KAEMPFEROL MARKER FROM EXTRACTS OF POINCIANELLA PYRAMIDALIS (TUL) L.P QUEIROZ

2017 ◽  
Vol 10 (12) ◽  
pp. 252
Author(s):  
Agna Heliade Oliveira ◽  
Valmir Gomesde Souza ◽  
FÁbio Santosde Souza ◽  
Rui Oliveira Macedo
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Herbal Medicines ◽  
Milling Process ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Limit Of Quantification ◽  
Development And Validation

Objective: This study aims to develop the extraction of the marker kaempferol in the fluid extract (FE) and validate an analytical method that monitors the quality of extracts of P. pyramidalis. Methods: The P. pyramidalis leaves were collected and then were dried to milling process. The extracts were drawn up at 20% weight: Volume (w/v) by maceration, and the extraction system used was hydroethanol solution ratio at 50:50 volume: Volume (v: v). From the hydroalcoholic extract, a method of extracting the kaempferol biomarker was developed and validated by high-performance liquid chromatography coupled with diode array detector. To validate a method, the following parameters were evaluated: Specificity, selectivity, linearity, limit of quantification (LOQ) and detection (LOD), precision, accuracy, robustness, and stability. Results: The method developed proved to be efficient, as it allowed the analysis of the interferents free marker, with recovery above 90%, linear over the range 1.4–26.6 μg/mL, correlation coefficient R2=0.999, and LOD and LOQ 0.07 and 0.22 μg/mL, respectively, specificity, precision, accuracy, and robustness. Conclusion: The extraction methodology of the kaempferol marker was successfully developed interferents free and the validated method by HPLC-DAD represents a useful tool in the quality control of P. pyramidalis herbal medicines.

Occurrence of Naphthalene in Honey Consumed in Turkey as Determined by High-Pressure Liquid Chromatography

2007 ◽  
Vol 70 (7) ◽  
pp. 1735-1738 ◽  
Author(s):  
DİREN BEYOĞLU ◽  
GÜLDEN Z. OMURTAG
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Signal To Noise ◽  
Limit Of Quantification ◽  
Naphthalene Concentration

This study is the first report on an investigation of the naphthalene concentration in samples of contaminated honey consumed in Turkey. Naphthalene was detected using high-performance liquid chromatography with a diode array detector at 220 nm. In one suspected contaminated specimen, the presence of naphthalene was confirmed by gas chromatography with mass spectrometry (GC-MS) at a concentration of 1.13 μg/kg. The limit of detection was 0.023 μg/g and the limit of quantification was 0.078 μg/g with signal-to-noise ratios of 3 and 10, respectively. A total of 100 samples of commercially available honey obtained from markets (53 samples) and street bazaars (47 samples) were analyzed. Mean naphthalene recovery from honey known to be contaminated with 1 μg/g was 80.4% (SD = 4.84%, n = 7).

scholarly journals Quantitative Determination by HPLC-DAD of Icariin, Epimedin A, Epimedin B, and Epimedin C in Epimedium (Berberidaceae) Species Growing in Turkey

2016 ◽  
Vol 11 (11) ◽  
pp. 1934578X1601101 ◽  
Author(s):  
Derya Cicek Polat ◽  
Maksut Coskun
Keyword(s):  
Quantitative Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Biologically Active ◽  
Array Detector ◽  
Diode Array ◽  
Gradient System ◽  
Diode Array Detector

The genus Epimedium is rich in terms of flavonoids, of which icariin, epimedin A, epimedin B and epimedin C are known especially to be biologically active. Therefore, it is important to quantify these compounds. In this study, a HPLC method coupled with DAD detection was developed and validated for the determination of icariin, epimedin A, epimedin B and epimedin C in Epimedium species growing in Turkey. The chromatographic separation was performed using a gradient system with a mobile phase of 0.1% formic acid (A) and acetonitrile (B) applied at a flow rate of 1 mL/min using a diode array detector. The highest values were, respectively, icariin 0.65%, epimedin A 0.13%, epimedin B 0.11%, epimedin C 0.06%. The highest values were obtained from the materials collected in Uzungol (Trabzon-Turkey).

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