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).

scholarly journals Quantitative Determination of Chemical Constituents from Seeds of Nigella sativa L. Using HPLC-UV and Identification by LC-ESI-TOF

2010 ◽  
Vol 93 (6) ◽  
pp. 1778-1787 ◽  
Author(s):  
Bharathi Avula ◽  
Yan-Hong Wang ◽  
Zulfiqar Ali ◽  
Ikhlas A Khan
Keyword(s):  
Nigella Sativa ◽  
Chemical Constituents ◽  
Hplc Method ◽  
Array Detector ◽  
Diode Array ◽  
Gradient System ◽  
Diode Array Detector ◽  
Column Material ◽  
Positive Ion

Abstract An HPLC method was developed for the simultaneous determination of nine compounds of Nigella sativa L. The separation was achieved within 23 min by using C18 column material, a wateracetonitrile mobile phase, both containing 0.1 acetic acid gradient system and a temperature of 35C. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ of nine compounds were in the range of 0.0910 and 0.325 g/mL, respectively. The wavelength used for quantification with the diode array detector was 205 and 260 nm. LC/MS coupled with electrospray ionization interface method is described for the identification of compounds in N. sativa L. samples. This method involved the use of [MH]<sup/> and [MNa]<sup/> ions in the positive ion mode with extracted ion chromatogram.

Analytical method for the determination of curcumin entrapped in polymeric micellar powder using HPLC

2021 ◽  
Vol 32 (4) ◽  
pp. 867-873
Author(s):  
Helmy Yusuf ◽  
Nina Wijiani ◽  
Rizka Arifa Rahmawati ◽  
Riesta Primaharinastiti ◽  
M. Agus Syamsur Rijal ◽  
...  
Keyword(s):  
Flow Rate ◽  
Analytical Method ◽  
Hplc Method ◽  
Array Detector ◽  
Good Resolution ◽  
Diode Array Detector ◽  
Accuracy And Precision ◽  
The Family ◽  
Effective Analysis

Abstract Objectives Curcumin belongs to the family of curcuminoids, natural polyphenolic compounds that possesses neuroprotective properties, anti inflammatory and anticancer. Its entrapment in the developed casein-based micellar powder (CMP) and poloxamer-based micellar powder (PMP) was to enhance the solubility and improve the bioavailability. Henceforth, the present study aimed to acquire an efficient analytical method for the curcumin analysis in polymeric micellar formulations. Methods A fast and specific HPLC method was developed for analyzing curcumin in two different micellar matrices using casein and poloxamer. The HPLC was equipped with a C18 column (250 × 4 mm, 5 µm) and diode array detector. A designated isocratic elution of curcumin was employed using mobile phase with a composition of water (1%, v/v acetic acid) and acetonitrile in a ratio of 50:50 v/v. The employed flow rate was 1.0 mL/min and the analyte was examined at 421 nm. Results An effective analysis in HPLC was successfully achieved by the predetermined HPLC condition. A good resolution of peaks at the employed flow rate was achieved. The linearity was excellent in two different range of concentrations, 2–20 and 10–50 μg/mL. The selectivity, accuracy and precision fulfilled the acceptable requirements. Conclusions The developed method was practically effective to qualitatively identified curcumin. In addition, the assay also effectively quantified the amount of curcumin in the polymeric entrapping matrices which demonstrates that it has great potential to be used in natural compound analysis.

scholarly journals Determination of Patulin in Apple Juice by Liquid Chromatography

2006 ◽  
Vol 89 (1) ◽  
pp. 139-143 ◽  
Author(s):  
Maria Helena Iha ◽  
Myrna Sabino
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Mobile Phase ◽  
Apple Juice ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Relative Standard ◽  
Precision Study

Abstract A method was developed and validated in-house for the determination of patulin (PAT), a toxic mold metabolite, in apple juice. The sample was extracted with ethyl acetatehexane and analyzed by liquid chromatography equipped with a C18 column and diode array detector. The mobile phase used for the quantification was waterethanol, at a flow rate of 0.5 mL/min. The method showed a mean recovery of 84.8%, the relative standard deviation obtained in the precision study was <7.7%, the quantification and detection limits were 7 and 3 μg/L, respectively, and the linear range for PAT in apple juice was 2.6650 μg/L. The ruggedness was evaluated by an intralaboratory experiment, in which 5 factors were studied, and only one was found to influence the observed results. The developed method is fast, practical, and simple; the solvents (except hexane) and reagents used were nontoxic. The results of the validation confirmed the efficiency of the method, which is sensitive enough to be used in studies required to quantify PAT in apple juice.

scholarly journals HPLC micromethod for amrinone and metabolites in patients receiving concurrent cephalosporin therapy

1996 ◽  
Vol 42 (5) ◽  
pp. 761-765
Author(s):  
J B Pappas ◽  
E M Allen ◽  
M Ross ◽  
W Banner
Keyword(s):  
Detection Limit ◽  
Mobile Phase ◽  
Sodium Phosphate ◽  
Hplc Method ◽  
Array Detector ◽  
Therapeutic Drug ◽  
Diode Array ◽  
Supernatant Fluid ◽  
Diode Array Detector ◽  
Sodium Phosphate Buffer

Abstract Amrinone (AMR), a bipyridine derivative, is receiving increasing use in postoperative cardiac patients as an inotrope and vasodilator. The hemodynamic response to amrinone in adults is linearly related to AMR concentrations, warranting therapeutic drug monitoring. We report a rapid microsample HPLC method for monitoring AMR and its principal metabolites, N-acetyl (N-ac) and N-glycolyl (N-gly) AMR. Serum was precipitated with acetonitrile, and the supernatant fluid was then injected into a C18 narrow-bore column. The mobile phase consisted of a 0.1 mol/L sodium phosphate buffer (pH 6) with a gradient of acetonitrile going from 50 to 100 mL/L of eluent. Detection with a diode-array detector (DAD) concurrently monitored the absorbances at 320 and 345 nm. Monitoring 320 nm allows optimal quantification of AMR, N-gly, and N-ac. Patients often receive concurrent cephalosporin therapy, which is detectable at 320 nm but not 345 nm. Because cephalosporins coelute with AMR or metabolites, monitoring at 345 nm allows separation of these antibiotics from AMR and metabolites while retaining a detection limit of 0.5 mg/L.

RP-LC Method for the Simultaneous Determination of Gliquidone, Pioglitazone Hydrochloride, and Atorvastatin in Formulations and Human Serum

2013 ◽  
Vol 96 (1) ◽  
pp. 56-59 ◽  
Author(s):  
Agha Zeeshan Mirza ◽  
M Saeed Arayne ◽  
Najma Sultana
Keyword(s):  
Phosphoric Acid ◽  
Quantitative Determination ◽  
Human Serum ◽  
Flow Rate ◽  
Drug Combination ◽  
Mobile Phase ◽  
Quantitative Method ◽  
Hplc Method ◽  
Established Method

Abstract The objective of this research was to develop and validate a rapid, economical, and sensitive HPLC method for quantitative determination of gliquidone, pioglitazone hydrochloride, and atorvastatin in tablets and serum. Due to drug combination of these formulations, there has been a need for a reliable quantitative method to determine these drugs in commercial samples and human serum. The chromatographic separation was carried out at ambient temperature with a mobile phase consisting of methanol–water (90 + 10, v/v), with pH adjusted to 3.50 with phosphoric acid. The pump was operated at a flow rate of 1 mL/min, and all analytes were detected at 235 nm. The method was linear over the concentration range of 5–50 μg/mL for all the drugs. The LOD of gliquidone, pioglitazone hydrochloride, and atorvastatin was 0.30, 1.30, and 0.57 μg/mL and LOQ was 0.98, 4.28, and 1.90 μg/mL, respectively. The proposed method was successfully applied to the determination of these drugs in commercial tablets and human serum. The established method was validated with respect to specificity, linearity, precision, accuracy, and ruggedness.

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.

scholarly journals Quantititative Determination of Lycorine and Galanthamine in Galanthus trojanus and G. cilicicus by HPLC-DAD

2014 ◽  
Vol 9 (8) ◽  
pp. 1934578X1400900
Author(s):  
Gulen Irem Kaya ◽  
Derya Cicek Polat ◽  
Buket Sarikaya ◽  
Mustafa Ali Onur ◽  
Nehir Unver Somer
Keyword(s):  
Biological Activities ◽  
Hplc Method ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Simple Method ◽  
Aerial Parts ◽  
Flowering Season ◽  
Low Mass

Lycorine and galanthamine have various biological activities. A reliable HPLC method coupled with DAD detection was developed and validated for the determination of galanthamine and lycorine in Galanthus trojanus and G. cilicicus. A simple method for the extraction of the alkaloids in low-mass plant samples was employed utilizing columns pre-packed with diatomaceous earth (Extrelut®). This method was applied to the aerial parts and bulbs of G. trojanus and G. cilicicus (Amaryllidaceae) collected during the flowering season. The chromatographic separation was performed using an isocratic system with a mobile phase of trifluoroacetic acid-water-acetonitrile (0.01:92.5:7.5) applied at a flow rate of 1 mL min−1 and using a diode array detector. Validation procedures showed that the method was specific, accurate and precise. The highest amount of lycorine (0.012%) was detected in the bulbs of G. trojanus collected from Çan (Çanakkale), whereas the aerial parts of this species collected from Bayramiç (Çanakkale) was not found to contain this alkaloid. In G. cilicicus samples, lycorine was only determined in the bulbs, giving yields of 0.004%; galanthamine yields were between 0.015-0.016%, but none of the G. trojanus samples contained this latter alkaloid.

scholarly journals Content of phenolic acids in rye caryopses determined using DAD-HPLC method

2013 ◽  
Vol 19 (No. 6) ◽  
pp. 201-205 ◽  
Author(s):  
R. Amarowicz ◽  
S. Weidner
Keyword(s):  
Phenolic Compounds ◽  
Phenolic Acids ◽  
Hplc Method ◽  
Uv Spectra ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Uv Spectrum ◽  
Free Phenolic Acids

Phenolic compounds were extracted from rye caryopses with 80% (v/v) methanol. Phenolic acids were determined as free compounds and those liberated from soluble esters and glycosides. The analyses were performed using a Waters HPLC system equipped with a diode array detector (DAD). The following free phenolic acids were found: p-coumaric, ferulic and sinapic; the phenolic acids liberated from soluble esters were as follows: vanillic, caffeic, p-coumaric, ferulic and sinapic; and those liberated from soluble glycosides were the following: vanillic, p-coumaric, ferulic and sinapic. In rye caryopses, phenolic acids were chiefly in the form of soluble esters. A diode array detector was especially useful for the determination of vanillic acid: the UV spectrum of this compound showed a maximum at 260 nm whereas UV spectra of other phenolic acids were characterised by maxima at longer wavelengths.

scholarly journals Detection of Impurities in a tablet of Atorvastatin

KYAMC Journal ◽  
2013 ◽  
Vol 1 (2) ◽  
pp. 43-47
Author(s):  
Mir Misbahuddin ◽  
Md. Saiful Islam ◽  
Uttam Kumar Sarker
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Bulk Drug

Identification of impurities and their amounts in the atorvastatin bulk drug and tablet DIVASTINTM (20 mg) were done using HPLC with diode array detector. The composition of mobile phase was acetonitril:phosphate buffer (45:55%; pH 4.0) with flow rate of 0.5 mL/min and detected at 248 ± 8 nm. Four impurities (desfluoro atorvastatin, distereoisomer, 3-o-methyl atorvastatin and lactone atorvastatin) were detected in the bulk drug whereas five impurities were detected in the tablet DIVASTINTM (20 mg). The total amounts of impurities in atorvastatin bulk drug and tablet were 0.804 and 0.983% respectively. In conclusion, the total amount of impurities was less than 1% which is acceptable.DOI: http://dx.doi.org/10.3329/kyamcj.v1i2.13313KYAMC Journal Vol.1(2) January 2011, 43-47

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