Automated Stopped-Flow Fluorimetric Sensor for Biologically Active Adamantane Derivatives Based on Zone Fluidics

A zone-fluidics (ZF) based automated fluorimetric sensor for the determination of pharmaceutically active adamantine derivatives, i.e., amantadine (AMA), memantine (MEM) and rimantadine (RIM) is reported. Discrete zones of the analytes and reagents (o-phthalaldehyde and N-acetylcysteine) mix and react under stopped-flow conditions to yield fluorescent iso-indole derivatives (λex/ λem = 340/455 nm). The proposed ZF sensor was developed and validated to prove suitable for quality control tests (assay and content uniformity) of commercially available formulations purchased from the Greek market (EU licensed) and from non-EU web-pharmacies at a sampling rate of 16 h−1. Interestingly, a formulation obtained through the internet and produced in a third—non-EU—country (AMA capsules, 100 mg per cap), was found to be out of specifications (mean assay of 85.3%); a validated HPLC method was also applied for confirmatory purposes.

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Determination of Oleanolic and Ursolic Acids in Sambuci flos Using HPLC with a New Reversed-phase Column Packed with Naphthalene Bounded Silica

Natural Product Communications ◽

10.1177/1934578x1701201206 ◽

2017 ◽

Vol 12 (12) ◽

pp. 1934578X1701201

Author(s):

Michal Gleńsk ◽

Maciej Włodarczyk

Keyword(s):

Oleanolic Acid ◽

Pharmacological Action ◽

Reversed Phase ◽

Hplc Method ◽

Biologically Active ◽

Factors Affecting ◽

New Type ◽

Phase Column ◽

Reversed Phase Column

Elder flowers have traditionally been used for their anti-inflammatory properties. However little is known about triterpenoid components in this Pharmacopoeial herbal drug. Herein, we report the quantification of ursolic and oleanolic acid in Sambuci flos by HPLC method. These biologically active triterpenoids were effectively separated and quantified using the elaborated HPLC chromatographic method with a naphthalene bounded silica reversed phase column. In this study, a very simple mobile phase for HPLC was developed to simultaneously determine both acids and the factors affecting separation were also discussed. The average content of oleanolic acid and ursolic acid in the elder flowers determined by proposed method was 2.06 mg/g and 11.56 mg/g respectively. This study showed both successful applications of the new type of reversed phase column and important contribution of mentioned triterpenoids to elder flower composition presumably resulting in its pharmacological action.

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Stability-Indicating HPLC Method for Determination of Naftazone in Tablets. Application to Degradation Kinetics and Content Uniformity Testing

Journal of Chromatographic Science ◽

10.1093/chrsci/49.7.495 ◽

2011 ◽

Vol 49 (7) ◽

pp. 495-501 ◽

Cited By ~ 7

Author(s):

M. I. Walash ◽

F. Belal ◽

N. El-Enany ◽

M. Eid ◽

R. N. El-Shaheny

Keyword(s):

Degradation Kinetics ◽

Hplc Method ◽

Content Uniformity ◽

Stability Indicating ◽

Content Uniformity Testing

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Determination of biologically active compounds (costunolide and dehydrocostuslactone) in the leaves of some forms of laurel noble (sweet bay)

IOP Conference Series Earth and Environmental Science ◽

10.1088/1755-1315/941/1/012015 ◽

2021 ◽

Vol 941 (1) ◽

pp. 012015

Author(s):

N M Nasukhova ◽

D A Konovalov ◽

V N Orobinskaya ◽

E V Galdin

Keyword(s):

Capillary Electrophoresis ◽

Sesquiterpene Lactones ◽

Hplc Method ◽

Biologically Active ◽

Economic Costs ◽

Plant Materials ◽

Crimean Peninsula ◽

Accuracy Of Results ◽

The Cost

Abstract Laurel noble (sweet bay) leaves are widely used for food (aromatic seasoning, preservative) and medicinal (antibacterial, anti-inflammatory, hepatoprotective) purposes. The plant is actively cultivated and has many ecological forms. The main sesquiterpene lactones in laurel leaves are costunolide and dehydrocostuslactone. The content of these substances varies significantly depending on the ecological-geographical, climatic, edaphic and other factors. Several methods have been developed and used to quantify these sesquiterpene lactones in laurel leaves. They differ significantly in the cost of equipment and materials required for research, the duration of the analysis, economic costs, and the accuracy of the results. The article presents the results of studying the content of costunolide and dehydrocostuslactone in the leaves of some forms of sweet bay, cultivated on the southern coast of the Crimean Peninsula using capillary electrophoresis methods, reliably confirmed by the results of HPLC analysis of the leaves of the studied forms of sweet bay. Studies have shown that both methods give comparable results. At the same time, the HPLC method is characterized by a higher accuracy of results and a lower determination error, and the method of capillary electrophoresis allows a study to be carried out with lower economic costs using simpler methods. Both methods are pharmacopoeial and are recommended for the standardization of medicinal plant materials.

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

Natural Product Communications ◽

10.1177/1934578x1601101110 ◽

2016 ◽

Vol 11 (11) ◽

pp. 1934578X1601101 ◽

Cited By ~ 1

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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Development and Validation of an Analytical Method for Deacetylasperulosidic Acid, Asperulosidic Acid, Scopolin, Asperuloside and Scopoletin in Fermented Morinda citrifolia L. (Noni)

Separations ◽

10.3390/separations8060080 ◽

2021 ◽

Vol 8 (6) ◽

pp. 80

Author(s):

Sun-Il Choi ◽

Hee-Yeon Kwon ◽

Im-Joung La ◽

Yeon-Hui Jo ◽

Xionggao Han ◽

...

Keyword(s):

Bioactive Compounds ◽

High Performance ◽

Limit Of Detection ◽

Hplc Method ◽

Biologically Active ◽

Morinda Citrifolia ◽

Coefficient Of Determination ◽

Analysis Method ◽

Food Ingredients

Fermentation is a technology that enhances biologically active ingredients, improves the absorption rate and induces the generation of new functional ingredients by the catalytic action of enzyme systems possessed by microorganisms. In this study, changes in the content of five kinds of bioactive compounds (deacetylasperulosidic acid, asperulosidic acid, scopolin, asperuloside and scopoletin) of Morinda citrifolia L. were confirmed by fermentation, and a high-performance liquid chromatography-photodiode array (HPLC-PDA) analysis method for measuring analytes was developed and validated. HPLC method for the determination of five bioactive compounds in Morinda citrifolia L. extracts (MCE) was validated in terms of sensitivity, linearity, selectivity, limit of detection (LOD) and quantification (LOQ), precision and accuracy. The coefficient of determination of the calibration curve for bioactive compounds (1.56–100 μg/mL) showed linearity (R2 ≥ 0.9999). LOD and LOQ were in the range 0.04–0.97 and 0.13–2.95 μg/mL, respectively. The range of intra- and intraday accuracies values (recovery) were 97.5–121.9% and 98.8–118.1%, respectively, and precision value (RSDs) of the bioactive compounds were <4%. In addition, changes in the content of five bioactive compounds in MCE by fermentation were confirmed. These results indicate that the developed fermentation and analysis method could be applied in the development of potential functional food ingredients.

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A Stability-Indicating HPLC Method for the Quantification of Aliskiren and Hydrochlorothiazide in a Pharmaceutical Formulation

Journal of AOAC International ◽

10.5740/jaoacint.13-383 ◽

2014 ◽

Vol 97 (6) ◽

pp. 1519-1525 ◽

Cited By ~ 3

Author(s):

Dimitrios Karvelis ◽

Eleni Kalogria ◽

Irene Panderi

Keyword(s):

Ammonium Acetate ◽

Degradation Products ◽

Hplc Method ◽

Percentage Error ◽

Forced Degradation ◽

Content Uniformity ◽

Isocratic Elution ◽

Stability Indicating ◽

Relative Percentage Error

Abstract A novel, fast, and sensitive stability-indicating HPLC method was developed, fully validated, and applied to the simultaneous determination of aliskiren and hydrochlorothiazide in a combined formulation. Effective chromatographic separation was achieved using a phenyl analytical column with isocratic elution using the mobile phase 0.030 M ammonium acetate–acetonitrile (60 + 40, v/v) at a flow rate of 0.40 mL/min. The UV spectrophotometric detector was set at 280 nm. The method was linear over the concentration ranges of 1.5–4.5 and 0.125–0.375 μg/mL for aliskiren and hydrochlorothiazide, respectively. The intraday and interday RSD values were less than 6.1%, while the relative percentage error, Er, was less than 5% for both analytes. Both drugs were subjected to stress conditions of acidic and alkaline hydrolysis, oxidation, and thermal degradation. The proposed method proved to be stability indicating by resolution of the drugs from their forced degradation products. The method was applied successfully to the QC and content uniformity tests in combined commercial tablets.

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ANALYTICAL METHOD DEVELOPMENT AND METHOD VALIDATION FOR DETERMINATION ASSAY AND CONTENT UNIFORMITY OF LEVONORGESTREL BY REVERSED-PHASE HIGHPERFORMANCE LIQUID CHROMATOGRAPHY

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2020.v13i4.36771 ◽

2020 ◽

pp. 101-107

Author(s):

Vikas kumar Pal ◽

Yogendra Pal

Keyword(s):

Liquid Chromatography ◽

Analytical Method ◽

Method Development ◽

Reversed Phase ◽

Hplc Method ◽

Acetonitrile Solution ◽

Simultaneous Estimation ◽

Content Uniformity ◽

Rp Hplc

Object: The main objective of the complete study is to develop a new method and also to validate the developed method for the determination of Assay and Content Uniformity of Levonorgestrel by reverse-phase high performance liquid chromatography (RP-HPLC). Methods: RP-HPLC method was developed for simultaneous estimation of levonorgestrel using Hypersil ODS, 125 mm×4.6 mm×5 μm C8 column with a mixture of water, and acetonitrile solution with a ratio of 50:50 as a mobile phase at a flow rate of 1.3 mL/min with a detection of quantification wavelength of 242 nm. Method was selected after calculating system suitability and validated as per International Conference on Harmonization (ICH) guidelines. Results: The developed analytical method parameters found within the limits as given in ICH and USP Guidelines and the total chromatographic analysis time per sample was 8 min with Levonorgestrel Eluting with retention time of 4.479, 4.479, and 4.467 min, respectively. The validated HPLC method was successfully applied for the determination of dissolution of levonorgestrel tablets. Conclusion: The method is simple, precise, specific, and accurate. The newly developed method can be used for routine analysis of Levonorgestrel in tablet dosage form.

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DETERMINATION OF AMINO ACIDS AND SUGARS CONTENT IN ANTENNARIA DIOICA GAERTN

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2019v11i5.33909 ◽

2019 ◽

pp. 39-43 ◽

Cited By ~ 2

Author(s):

LIUDMYLA SLOBODIANIUK ◽

LILIIA BUDNIAK ◽

SVITLANA MARCHYSHYN ◽

ROXOLANA BASARABA

Keyword(s):

Amino Acids ◽

Free Amino ◽

Hplc Method ◽

Biologically Active Substances ◽

Biologically Active ◽

New Drugs ◽

Raw Material ◽

Primary Metabolites ◽

Active Substances

Objective: The purpose of our study was to determine sugars and amino acids content of Antennaria dioica Gaertn. herb. In continuation of the investigation of biologically active substances from Antennaria dioica Gaertn., it advisable to study the qualitative composition and quantitative contents of sugars and amino acids from the herb of this plant. Methods: The herb of Antennaria dioica Gaertn. was analyzed for the content of sugars by GC/MS. The amino acids were identified and quantified by HPLC method. Results: The results of GC/MS analysis showed that in Antennaria dioica Gaertn. herb D-glucose had the highest content (7.16±0.09) mg/g, followed by D-fructose (5.27±0.06) mg/g and D-saccharose (6.72±0.08) mg/g. In the raw material a large amount of monosaccharides derivative–Myo-inositol was revealed, a content of which was (2.12±0.06) mg/g. We determined 17 bound and 16 free amino acids in the Antennaria dioica Gaertn. by HPLC method. Conclusion: The contents of primary metabolites provide opportunities for creating medicine and food supplements. The results show that Antennaria dioica Gaertn. is a rich source of these important biologically active substances. The resulting data will be used with the further purpose to produce new drugs of natural origin.

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