scholarly journals Rapid Determination of α-Hederin and Hederacoside C in Extracts of Hedera helix Leaves Available in the Czech Republic and Poland

2015 ◽  
Vol 10 (9) ◽  
pp. 1934578X1501000
Author(s):  
Lucie Havlíková ◽  
Kateřina Macáková ◽  
Lubomír Opletal ◽  
Petr Solich
Keyword(s):  
Mobile Phase ◽  
Ammonium Acetate ◽  
Rapid Determination ◽  
Hplc Method ◽  
Leaf Extracts ◽  
Hedera Helix ◽  
The Czech Republic ◽  
Upper Respiratory ◽  
Isocratic Mode

Leaf extracts of Hedera helix L. are widely used in the treatment of upper respiratory diseases. The saponins α-hederin and hederacoside C are considered to be the main compounds responsible for the biological activity. α-Hederin and hederacoside C were determined in H. helix leaf extracts using a fast, simple and validated HPLC method. An XTerra MS C18 column and mobile phase composed of 10 mM ammonium acetate at pH 8.5 (adjusted with triethylamine) and acetonitrile were used for the chromatography at 1.2 mL min−1. The column was kept at 30°C. Detection was performed at 220 nm. An approach utilizing a basic pH of the aqueous part of the mobile phase enabled analysis in 5 minutes in isocratic mode. The method was validated and used for the quality control of H. helix leaf ethanolic extracts.

scholarly journals Development of a Method to Determine Albendazole and Its Metabolites in the Muscle Tissue of Yellow Perch Using High-Performance Liquid Chromatography with Fluorescence Detection

2011 ◽  
Vol 94 (2) ◽  
pp. 446-452 ◽  
Author(s):  
Donglei Yu ◽  
Nathan Rummel ◽  
Badar Shaikh
Keyword(s):  
High Performance Liquid Chromatography ◽  
Muscle Tissue ◽  
Mobile Phase ◽  
Yellow Perch ◽  
High Performance ◽  
Ammonium Acetate ◽  
Hplc Method ◽  
Tissue Samples ◽  
Phase Combination

Abstract An HPLC method was developed for the determination of albendazole (ABZ) and its metabolites, a sulfoxide (ABZSO), a sulfone (ABZSO2), and albendazole-2-aminosulfone (ABZ-2-NH2SO2), from yellow perch muscle tissue with adhering skin. The muscle tissue samples were made alkaline with potassium carbonate and extracted with ethyl acetate, followed by a series of liquidliquid extraction steps. After solvent evaporation, the residue was reconstituted in the initial mobile phase combination of the gradient. The mobile phase consisted of a buffer, 50 mM ammonium acetate (pH 4.0) in 10 methanolwater, and 100 acetonitrile. The gradient was from 20 acetonitrile to 85 acetonitrile. The analytes were chromatographed on an RP Luna C18(2) column and detected by fluorescence with excitation and emission wavelengths of 290 and 330 nm, respectively. The average recoveries from fortified muscle tissue for ABZ (20100 ppb), ABZ-SO (20200 ppb), ABZSO2 (8100 ppb), and ABZ-2-NH2SO2 (20100 ppb) were 85, 95, 101, and 86, respectively, with corresponding CV values of 9, 3, 6, and 4, respectively. Their LOQ values were 10, 10, 1, and 10 ppb, respectively. The procedure was applied to determine ABZ and its major metabolites in the incurred muscle tissue of yellow perch obtained after orally dosing the fish with ABZ.

scholarly journals APPLICATION OF VALIDATED RP-HPLC METHOD FOR THE DETERMINATION OF ARMODAFINIL IN BULK AND FORMULATION

2017 ◽  
pp. 158-161
Author(s):  
Devi Ramesh ◽  
Mohammad Habibuddin
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Isocratic Mode

Objective: The objective of the present study is to develop and validate a simple, rapid, sensitive reverse phase HPLC method for the determination of Armodafinil present in bulk and its pharmaceutical formulations.Methods: The chromatographic separation was achieved by using Hypersil ODS C-18 (150 x 4.6 mm, 5µ) in an isocratic mode with mobile phase methanol: phosphate buffer 3.0 (60:40 %v/v) was used. The flow rate was 1 ml/min and effluent was monitored at 225 nm. The method was validated for validation parameters i.e. linearity, accuracy, precision and robustness according to ICH guidelines.Results: The retention time of Armodafinil was 4.2 min and the linearity range of the method was 500-20000ng/ml with regression (r2) coefficient 0.9998. The method was validated for precision, accuracy, robustness and which were found to be within the acceptable limits according to the ICH guidelines. Also, the method was successfully applied for the estimation of Armodafinil in the marketed formulation of Nuvigil and the recovery was found to be>98%.Conclusion: The developed method possess good selectivity, specificity, there is no interference found in the blank at a retention time of ARM and good correlation between the peak area and concentration of the drugs under prescribed conditions. Hence, the method can be applied for routine analysis of Armodafinil. 

Method for the Determination of Catechin and Epicatechin Enantiomers in Cocoa-Based Ingredients and Products by High-Performance Liquid Chromatography: Single-Laboratory Validation

2012 ◽  
Vol 95 (2) ◽  
pp. 500-507 ◽  
Author(s):  
Philip R Machonis ◽  
Matthew A Jones ◽  
Brian T Schaneberg ◽  
Catherine L Kwik-Uribe
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chiral Stationary Phase ◽  
Ammonium Acetate ◽  
Hplc Method ◽  
Routine Laboratory ◽  
Performance Results ◽  
Single Laboratory ◽  
Monomeric Flavanols

Abstract A single-laboratory validation study was performed for an HPLC method to identify and quantify the flavanol enantiomers (+)- and (–)-epicatechin and (+)- and (–)-catechin in cocoa-based ingredients and products. These compounds were eluted isocratically with an ammonium acetate–methanol mobile phase applied to a modified β-cyclodextrin chiral stationary phase and detected using fluorescence. Spike recovery experiments using appropriate matrix blanks, along with cocoa extract, cocoa powder, and dark chocolate, were used to evaluate accuracy, repeatability, specificity, LOD, LOQ, and linearity of the method as performed by a single analyst on multiple days. In all samples analyzed, (–)-epicatechin was the predominant flavanol and represented 68–91% of the total monomeric flavanols detected. For the cocoa-based products, within-day (intraday) precision for (–)-epicatechin was between 1.46–3.22%, for (+)-catechin between 3.66–6.90%, and for (–)-catechin between 1.69–6.89%; (+)-epicatechin was not detected in these samples. Recoveries for the three sample types investigated ranged from 82.2 to 102.1% at the 50% spiking level, 83.7 to 102.0% at the 100% spiking level, and 80.4 to 101.1% at the 200% spiking level. Based on performance results, this method may be suitable for routine laboratory use in analysis of cocoa-based ingredients and products.

Determination of Residues of Acetaminophen, Caffeine, and Drotaverine Hydrochloride on Swabs Collected from Pharmaceutical Manufacturing Equipment Using HPLC in Support of Cleaning Validation

2014 ◽  
Vol 97 (5) ◽  
pp. 1439-1445 ◽  
Author(s):  
Mohamed E M Hassouna ◽  
Yousry M Issa ◽  
Ashraf G Zayed
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Pharmaceutical Manufacturing ◽  
Manufacturing Equipment ◽  
Cleaning Validation ◽  
Accuracy And Precision ◽  
Drotaverine Hydrochloride ◽  
Time Required ◽  
Isocratic Mode

Abstract An HPLC method was developed for the simultaneous determination of residues of acetaminophen (paracetamol, PA), caffeine (CA), and drotaverine HCl (DH) on swabs collected from pharmaceutical manufacturing equipment surfaces. The challenge in cleaning validation is to develop analytical methods that are sensitive enough to detect traces of the active compounds remaining on the surface of pharmaceutical manufacturing equipment after cleaning. Chromatography was performed in the isocratic mode on a Hypersil C18 BDS column using the mobile phase 0.02 M tetrabutylammonium bisulfate–methanol (100 + 45, v/v) at 50°C with UV detection at 210 nm. The method was tested for specificity, linearity, LOD, LOQ, accuracy, and precision for determination of traces of the above-mentioned drugs. The time required for a single analysis was 12 min. The response was linear in the ranges of 6.900–52.100, 1.040–7.800, and 0.694–5.210 μg/mL for PA, CA, and DH, respectively.

scholarly journals Simultaneous Quantification of Hederacoside C and α-hederin in Hedera Nepalensis K.Koch Using HPLC-UV

2020 ◽  
Vol 36 (3) ◽  
Author(s):  
Do Thi Thuy Linh ◽  
Hoang Thanh Duong ◽  
Nguyen Tuan Hiep ◽  
Pham Thanh Huyen ◽  
Nguyen Minh Khoi ◽  
...  
Keyword(s):  
Medicinal Plants ◽  
Rapid Determination ◽  
Publishing House ◽  
Leaf Extracts ◽  
Hedera Helix ◽  
Dipeptidyl Peptidase 4 ◽  
Simultaneous Quantification ◽  
Study Results

 This study develops a high performance liquid chromatography with ultraviolet detection (HPLC-UV) for simultaneous quantification of hederacoside C and α-hederin in Hedera nepalensis K. Koch. The method proposed in this study was validated in terms of the analytical parameters such as high repeatability, high accuracy and good sensitivity. The method was used to determine the content of hederacoside C and α-hederin in Hedera nepalensis K. Koch, which had been collected in Ha Giang, Lao Cai and Lai Chau. The study results show that the content of hederacoside C and the content of α-hederin ranged from 0.40 to 4.01% and 0.21 – 0.54% based on absolute dry mass, respectively. Keywords Hedera nepalensis K. Koch, hederacoside C, α-hederin, HPLC-UV. References [1] L. Jafri, et al, In vitro assessment of antioxidant potential and determination of polyphenolic compounds of Hedera nepalensis K. Koch, Arabian Journal of Chemistry. 10 (2017) 3699-3706. https://doi.org/10.1016/j.arabjc.2014.05.002.[2] S. Saleem, et al, Plants Fagonia cretica L, and Hedera nepalensis K. Koch contain natural compounds with potent dipeptidyl peptidase-4 (DPP-4) inhibitory activity, Journal of ethnopharmacology. 156 (2014) 26-32. https://doi.org/10.1016/j.jep.2014.08.017[3] D.H. Bich, Medicinal plants and animals for medicine in Vietnam, Vol 1, Science and Technics Publishing House, Hanoi, 2006 (in Vietnamese).[4] National Institute Of Medicinal Materials, List of medicinal plants in Vietnam, Science and Technics Publishing House, Hanoi, 2016 (in Vietnamese).[5] L. Jafri, et al, Hedera nepalensis K. Koch: A Novel Source of Natural Cancer Chemopreventive and Anticancerous Compounds, Phytotherapy research. 30(3) (2016) 447-453. https://doi.org/10.1002/ptr.5546. [6] S. Kanwal, et al, Antioxidant, antitumor activities and phytochemical investigation of Hedera nepalensis K. Koch, an important medicinal plant from Pakistan, Pakistan Journal of Botany. 43 (2011) 85-89. [7] G. Uddin, et al, Biological screening of ethyl acetate extract of Hedera nepalensis stem, African Journal of Pharmacy and Pharmacology. 6(42) (2012) 2934-2937. https://doi.org/10.5897/AJPP12.828 [8] H. Kizu, et al, Studies on Nepalese Crude Drugs, III, On the Saponins of Hedera nepalensis K. Koch, Chemical and Pharmaceutical Bulletin. 33(8) (1985) 3324-3329. https://doi.org/0.1248/cpb.33.3324[9] X. Tong, et al, Extraction and GC-MS Analysis of Volatile Oil from Hedera nepalensis var sinensis, Fine Chemicals. 24(6) (2007) 559-561. [10] EDQM, European Pharmacopoeia, fifth ed., Council of Europe, France, 2015. [11] N.T.H. Mai, et al, Simultaneous Quantification of Hederacoside C and α-Hederin from the Leaves of Hedera helix L. by HPLC, Journal of Medicinal Material. 21(6) (2016). (in Vietnamese).[12] L. Havlíková, et al, Rapid Determination of α-Hederin and Hederacoside C in Extracts of Hedera helix Leaves Available in the Czech Republic and Poland, Natural product communications. 10(9) (2015). https://doi.org/10.1177/1934578X1501000910[13] M. Yu, et al, Determination of Saponins and Flavonoids in Ivy Leaf Extracts Using HPLC-DAD, Journal of Chromatographic Science. 53(4) (2014) 478-483. https://doi.org/10.1093/chromsci/bmu068.[14] EMEA, Validation of analytical procedures: text and methodology Q2 (R1), in International conference on harmonization, Geneva, Switzerland, 2005. [15] W. Horwitz, Official methods of analysis, 12 ed., Vol 1, Association of Official Analytical Chemists, Washington DC, 1975.

scholarly journals DEVELOPMENT AND VALIDATION OF A HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD DETERMINATION OF ZIDOVUDINE ENCAPSULATED IN PCL NANOPARTICLES

2017 ◽  
Vol 1 (2) ◽  
pp. 1-8
Author(s):  
Milena Cristina Ribeiro Souza Magalhães ◽  
Alisson Samuel Portes Caldeira ◽  
Hanna De Sousa Rocha Almeida ◽  
Sílvia Ligório Fialho ◽  
Armando Da Silva Cunha Junior
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Isocratic Mode

A reversed-phase high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of encapsulation efficiency of zidovudine in nanoparticules. The method was carried out in isocratic mode using 0.040M sodium acetate: methanol: acetonitrile: glacial acetic acid (880:100:20:2) as mobile phase, a C8 column at 25ºC and UV detection at 240 nm. The method was linear (r2 ˃ 0.99) over the range of 25.0-150.0 μg/mL, precise (RSD ˂ 5%), accurate (recovery = 100.5%), robust and selective. The validated HPLC-UV method can be successfully applied to determine the rate of zidovudine in nanoparticules.

A SIMPLE AND RAPID HPLC METHOD FOR ESTIMATION OF DIMETHICONE FROM FORMULATIONS

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (03) ◽  
pp. 26-29
Author(s):  
J. J Jadhav ◽  
◽  
S Mungekar ◽  
J. V. Velada ◽  
H. A. Doshi ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Forms ◽  
Hplc Method ◽  
Normal Phase ◽  
Hplc Separation ◽  
Tablet Dosage ◽  
Refractive Index Detector ◽  
Isocratic Mode

A simple, sensitive, precise and specific normal phase high performance liquid chromatography (HPLC) method was developed and validated for the determination of dimethicone from tablet dosage forms. It was found that the excipients used in the tablet dosage form did not interfere in the quantification of dimethicone. The HPLC separation was carried out by normal phase chromatography on Princeton Sphere Cyano, 250 x 4.6mm, 5µ with a mobile phase composed of hexane : ethanol : ethyl acetate (80:20:0.2) in isocratic mode at a flow rate of 0.5mL/min. Dimethicone was quantified using a refractive index detector. The calibration curve for dimethicone was linear from 1.75 to 3.25 mg/mL. The inter-day and intra-day precisions were found to be within limits. The proposed method has adequate sensitivity, reproducibility and specificity for the determination of dimethicone from tablet dosage forms.

Rapid Determination of Metronidazole and 2-Hydroxymetronidazole in Murine Blood Plasma

2021 ◽  
Author(s):  
Nina Zemanová ◽  
Pavel Anzenbacher ◽  
Tomáš Hudcovic ◽  
Eva Anzenbacherová
Keyword(s):  
Plasma Proteins ◽  
Mobile Phase ◽  
High Performance ◽  
Rapid Determination ◽  
Internal Standard ◽  
Hplc Method ◽  
Primary Metabolite ◽  
Relative Standard ◽  
Protozoan Infections

Abstract Metronidazole is a drug used to treat bacterial and protozoan infections. Nowadays, it is one of the most frequently prescribed drugs worldwide. The main aim of this paper is to present a rapid, reliable and simple high-performance liquid chromatography (HPLC) method to determine metronidazole along with its primary metabolite, 2-hydroxymetronidazole, in plasma or serum using paracetamol as an internal standard. A total of 100% methanol was used to denature plasma proteins. After centrifugation, the supernatant was evaporated under nitrogen flow. The samples were dissolved in the mobile phase and injected into a Li-Chrospher RP-18 column. A total of 10 mmol/L NaH2PO4: acetonitrile (90:10, v/v) solution with a flow rate of 1 mL/min was used as the mobile phase. Metronidazole and 2-hydroxymetronidazole were detected at two different wavelengths at 320 nm and 311 nm, respectively. The method is characterized by high precision (relative standard deviation % < 6). The method was used for the determination of metronidazole and 2-hydroxymetronidazole in murine blood using small amounts of plasma (≤100 μL).

scholarly journals Quantitative analysis of Loperamide hydrochloride in the presence its acid degradation products

2009 ◽  
Vol 63 (1) ◽  
pp. 39-46 ◽  
Author(s):  
Ivana Savic ◽  
Goran Nikolic ◽  
Ivan Savic ◽  
Valentina Marinkovic
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Rapid Determination ◽  
Parent Compound ◽  
Ammonium Hydroxide ◽  
High Sensitivity ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Acid Degradation

The aim of this work was to develop a new RP-HPLC method for the determination of loperamide hydrochloride in the presence of its acid degradation products. Separation of loperamide from degradation products was performed using ZORBAX Eclipse XDB C-18, column with a mobile phase consisting of 0.1% sodium-octansulphonate, 0.05% triethylamine, 0.1% ammonium hydroxide in water:acetonitrile (45:55 v/v). The mobile phase was adjusted to pH 3.2 with phosphoric acid. The method showed high sensitivity with good linearity over the concentration range of 10 to 100 ?g cm-3. The method was successfully applied to the analysis of a pharmaceutical formulation (Loperamide, Zdravlje-Actavis, Serbia) containing loperamide hydrochloride with excellent recovery. The loperamide hydrochloride degradation during acid hydrolysis and kinetics investigation was carried out in hydrochloric acid solutions of 0.1, 1.0 and 1.5 mol dm-3, at different temperatures (25 and 40?C), by monitoring the parent compound itself. The first order reaction of loperamide degradation in acid solution was determined. The activation energy was estimated from the Arrhenius plot and it was found to be 38.81 kJ mol-1 at 40?C. The developed procedure was successfully applied for the rapid determination of loperamide hydrochloride in pharmaceutical formulation (Loperamide, Zdravlje-Actavis, Serbia) and in the presence of its acid degradation products.

Multivariate Optimization of Separation Conditions for Simultaneous Determination of Acemetacin and Chlorzoxazone in a Pharmaceutical Preparation by HPLC Using Response Surface Methodology

2013 ◽  
Vol 96 (4) ◽  
pp. 723-729
Author(s):  
Cigdem Aybaba ◽  
Ismail Murat Palabiyik ◽  
Mehmet Gokhan Caglayan ◽  
Feyyaz Onur
Keyword(s):  
Response Surface Methodology ◽  
Response Surface ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
Ammonium Acetate ◽  
Pharmaceutical Preparation ◽  
Internal Standard ◽  
Hplc Method ◽  
Optimum Separation

Abstract A new, fast, accurate, precise, and sensitive RP-HPLC method for the simultaneous determination of acemetacin and chlorzoxazone has been developed. Response surface methodology with a central composite design was used to optimize the acetonitrile and ammonium acetate percentage in the mobile phase and pH of ammonium acetate. The optimum separation was achieved on a C18 column (250 × 4.6 mm id, 5 μm particle size) using the mobile phase methanol–acetonitrile–0.02 M ammonium acetate, pH 9.4 (25 + 35 + 40, v/v/v) at a flow rate of 1.5 mL/min; UV detection at 270 nm, and cyanocobalamin as an internal standard. This developed method was validated and successfully applied to a coated tablet pharmaceutical preparation.

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