Validation of Metamizole, Thiamin and Pyridoxine Simultaneous Analysis Methods in Tablet Preparations Using HPLC

The aim of the present study was to develop and validate HPLC method for the simultaneous assay of metamizole, thiamine and pyridoxine in tablet. Metamizole is a substance that is easily hydrolyzed in the precence of water and oxygen. To inhibit the hydrolysis of metamizole during sample preparation prior to HPLC analysis, sodium sulfite is added and its optimum concentration was investigated. The chromatographic system includes a RP C8(2) column (150x4.6 mm, 5 µm particle size) in conjunction with Photo Diode Array (PDA) detector. The optimal chromatographic condition was obtained using a mobile phase consisting of phosphate buffer 35mM pH 3.0: methanol (80:20), flowrate 1.0 ml/min, and 10 µl injection volume. The metamizole, thiamine and pyridoxine were detected at 275 nm and 361 nm for cyanocobalamin. The Hydrolysis of metamizole was successfully inhibited by adding solution containing 1.5 mg/mL sodium sulfite to solvent and 0.5 mg/mL sodium sulfite to mobile phase. The validation results indicate a good specificity and a linear detector responses with r>0.999. The accuracy (% recovery) for metamizole, thiamine and piridoxine were 100.26%; 99.09%; and 100.03%, respectively. The method yields good precision with RSD of metamizole, thiamine and pyridoxine were 2.0912%; 1.4489%; and 0.8418% respectively. In the robustness study, the small changes of mobile phase pH yielded unsymmetrical peaks and lower resolution. The validated method was successfully applied for simultaneous assay of metamizole, thiamine and pyridoxine in tablet. Keywords: validation; metamizole; thiamine; pyridoxine; hydrolysis of metamizole; HPLC

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

Clinical Chemistry ◽

10.1093/clinchem/42.5.761 ◽

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.

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Phenobarbital Analysis in Biological Matrix (Blood) by High Performance Liquid Chromatography (HPLC)

International Letters of Chemistry Physics and Astronomy ◽

10.18052/www.scipress.com/ilcpa.20.31 ◽

2013 ◽

Vol 20 ◽

pp. 31-40

Author(s):

Ouakouak Hamza ◽

Ben Mohamed Moktar ◽

Ben Chohra Mostafa ◽

Abdelhamid Zeghdaoui

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Mobile Phase ◽

High Performance ◽

Ammonium Acetate ◽

Analytical Techniques ◽

Hplc Method ◽

Diode Array ◽

Blood Components ◽

Ammonium Acetate Buffer

In this work, we have tried to contribute to the analysis of phenobarbital in the blood. To do this, we used different analytical techniques such as liquid chromatography (HPLC). The results obtained in the course of our work, we can conclude that: The HPLC method was separate phenobarbital endogenous blood components, and optimizing the conditions of chromatographic separation as the composition of the mobile phase consisting of 20% acetonitrile + 20% methanol + 60% ammonium acetate buffer. The extraction with diethyl ether to pH = 4; The chromatographic column, microbondapack ZORBAX C18. A system of diode-array UV detection at 254 nm.

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Daidzein and genistein concentrations in human milk after soy consumption

Clinical Chemistry ◽

10.1093/clinchem/42.6.955 ◽

1996 ◽

Vol 42 (6) ◽

pp. 955-964 ◽

Cited By ~ 88

Author(s):

A A Franke ◽

L J Custer

Keyword(s):

Human Milk ◽

Ethyl Acetate ◽

Electrochemical Detection ◽

Newborn Infants ◽

Hplc Method ◽

Soy Isoflavones ◽

Spectrometric Analysis ◽

Diode Array ◽

Array Detection ◽

Hydrolysis Of

Abstract Soy isoflavones were quantified from human milk by a fast, precise, and selective HPLC method after enzymatic hydrolysis of conjugated isoflavones and extraction with ethyl acetate. Isoflavone aglycones and their mammalian metabolites equol and O-desmethylangolensin were separated selectively and identified by absorbance patterns, fluorometric and electrochemical detection, gas chromatography-mass spectrometric analysis after trimethylsilylation, and with internal and external authentic standards. HPLC injections of 20 microL of human milk showed detection limits of 1-3 pmol for all analytes by using diode-array detection. The detection limit could be improved by as much as 1000-fold by extended concentration through partitioning with ethyl acetate, by using electrochemical detection, by increasing the injection volumes, or by combining these techniques. We used the proposed method to monitor isoflavone concentrations in human milk and in human urine after challenge with 5, 10, and 20 g of roasted soybeans in the diet. Implications of the results for the potential of isoflavones to prevent cancer in newborn infants exposed to these agents are discussed.

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QBD APPROACH TO ANALYTICAL METHOD DEVELOPMENT AND ITS VALIDATION FOR ESTIMATION OF LENVATINIB IN BULK AND PHARMACEUTICAL FORMULATION

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2021v13i5.41786 ◽

2021 ◽

pp. 183-188

Author(s):

SACHIN A. BABAR ◽

SUDHAKAR L. PADWAL

Keyword(s):

Central Composite Design ◽

Mobile Phase ◽

High Performance ◽

Method Development ◽

Hplc Method ◽

Factor Screening ◽

Pharmaceutical Dosage Forms ◽

Rp Hplc ◽

Chromatographic Condition ◽

Central Composite

Objective: The objective of this research was to develop a simple, very rapid, sensitive, accurate, precise reverse phase High-Performance Liquid Chromatography (RP-HPLC) technique for the estimation of Lenvatinib in bulk and its dosage form. Methods: To perform this study, we employed a central composite design (CCD) to make method robust and effective to create chromatographic database. The factor screening studies were performed using 2-factor 10-runs. The factors were selected as the mobile phase ratio and buffer pH. Results: The desirability value of the optimized model was found to be 0.869 and The optimized chromatographic condition was achieved on Enable C18 analytical column with 0.01M Ammonium acetate buffer pH 3.84: methanol (33.17:66.83 v/v) as the mobile phase and flow rate of 1 ml min-1 and detection wavelength was set to 240 nm. The retention time of Lenvatinib was found to be 5.122 min. Linearity was established for Lenvatinib in the range of 10-50 µg/ml with a correlation coefficient (r2=0.9995). The accuracy values were found to be in the range of 98–102%. Intraday precision and Interday precision were in prescribed (Less than 0.98% RSD). Robustness was found to be less than 1.22% RSD. Conclusion: The proposed method was useful for best analysis of Lenvatinib in Bulk pharmaceutical dosage forms. Central Composite Design was an effective tool for the proposed RP-HPLC method.

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STUDI PERBANDINGAN ANALISIS VITAMIN E MINYAK SAWIT MERAH TERSAPONIFIKASI ANTARA METODE SPEKTROFOTOMETRI UV-VIS DAN KCKT

KOVALEN ◽

10.22487/j24775398.2017.v3.i1.8233 ◽

2017 ◽

Vol 3 (1) ◽

pp. 50

Author(s):

Arlina Mayharty Andulaai ◽

Ruslan Ruslan ◽

Hardi Ys. ◽

Dwi Juli Puspitasari

Keyword(s):

High Performance Liquid Chromatography ◽

Vitamin E ◽

Palm Oil ◽

Mobile Phase ◽

High Performance ◽

Hplc Analysis ◽

Ultra Violet ◽

Hplc Method ◽

Red Palm Oil ◽

Extraction Spectrophotometry

A research about a comparative study of spectrophotometry UV-Vis and HPLC method for the analysis of vitamin E in saponified red palm oil has been done. This research aims to compare the results of analysis using Spectrophotometer UV - Vis and HPLC to determine the concentration of vitamin E in red palm oil previously saponified and extracted. HPLC analysis was carried out using an RP-18 column and mobile phase composed a methanol and water ( 86:14 ), with a flow rate of 1 ml/min and UV detection at 290 nm. For the Spectrophotometric UV-Vis analysis, hexane was used as a solvent and the wavelength at 298,5 nm was selected for the detection. The results are the concentration of vitamin E using spectrophotometric and HPLC method was respectively 104.5 ppm and 127 ppm.Keyword: Vitamin E, Red Palm Oil, saponification, extraction, spectrophotometry Ultra Violet -Visible, High Performance Liquid Chromatography

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Hydrolysis, alcoholysis and aminolysis of N,N'-malonyldiimidazole

Butlerov Communications ◽

10.37952/roi-jbc-01/19-58-6-49 ◽

2019 ◽

Vol 58 (6) ◽

pp. 49-54

Author(s):

Pyotr P. Purygin ◽

◽

Vitaly Yu. Alekseev ◽

Ekaterina A. Agapova ◽

Yury P. Zarubin ◽

...

Keyword(s):

Mobile Phase ◽

Kinetic Studies ◽

Hplc Method ◽

High Reactivity ◽

Biologically Active ◽

Acyl Residue ◽

Elimination Mechanism ◽

Condensing Agents ◽

Kinetics Of ◽

Hydrolysis Of

The achievements of molecular biology, biochemistry and bioorganic chemistry are largely due to the methods of organic chemistry, in particular chemistry N-azolides over the past twenty years. Imidazolides are not the most reactive group of compounds among heterocyclic amides, however, it is interesting for preparative purposes because of the availability of imidazole. It is known that compounds of this class are widely used as specific condensing agents in the synthesis of a number of biologically active substances. The investigation of the physicochemical properties of N-azolides is of great interest. According to well-known kinetic studies, the aminolysis and the alcoholysis of N-azolides proceed according to the addition-elimination mechanism. The hydrolysis of N-azolides of sterically hindered carboxylic acids proceeds according to the mechanism of monomolecular nucleophilic substitution. These conclusions are based on the study of the dependence of the rate constants and the activation energy of the acyl residue. Differences in the reactivity of N-azolides with different acyl residues are quite pronounced. In this work, the reactions of hydrolysis, alcoholysis and aminolysis of N,N'-malonyldiimidazole were studied by an HPLC method on an isocratic pump chromatograph, with a UV spectrophotometric detector with a wavelength range of 190–600 nm. A polar chromatographic column with a particle size of 5 μm was used. Acetonitrile eluent (CH3CN) was used as the mobile phase. The speed of the mobile phase was 1,000 ml/min. Before the experiment, air was removed from the mobile phase by degassing into an ultrasonic bath. We used the program "Open LAB" for processing the results. Chromatography was carried out in isocratic mode at a wavelength of 280 nm. After a certain period of time, chromatography was carried out and a decreasing peak area of the starting dionicid of malonic acid was noted. The kinetics of the processes of hydrolysis, aminolysis of alcoholysis was determined during the study. The relative instability of N,N'-malonyldiimidazole and high reactivity were established because of the calculated half-life data.

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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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Tannins Compound In Soga Tingi Bark (Ceriops Tagal) As Natural Dyes

EKUILIBRIUM Journal of Chemical Engineering ◽

10.20961/equilibrium.v5i1.48505 ◽

2021 ◽

Vol 5 (1) ◽

pp. 1

Author(s):

Paryanto Paryanto ◽

Sunu Herwi Pranolo ◽

Ari Diana Susanti ◽

Bintang Timur Putrikatama ◽

I. R. Qatrunada ◽

...

Keyword(s):

Textile Industry ◽

Mobile Phase ◽

Hplc Analysis ◽

Hplc Method ◽

Natural Dyes ◽

Ftir Analysis ◽

Tannin Content ◽

Textile Materials ◽

Ceriops Tagal ◽

Guava Leaf

In general, natural dyes for textile materials are obtained from extracts part of the plants such as roots, wood, leaves, seeds, and flower. Textile industry especially batik craftsman, have known many plants that can dye textile materials, such as indigo (indigofera), soga tingi bark (Ceriops tagal), tegeran wood (Cudraina javanensis), turmeric (Curcuma), tea (The), noni root (Morinda citrifelia), soga jambal bark (Pelthophorum ferruginum), kesumba (Bixa orelana), and guava leaf (Psidiumguajava). Soga tingi bark chosen because it can produce tannins which can be used as natural dyes. The purpose of this research was to obtained tannin content in soga tingi bark as qualitatively and quantitatively. The analysis carried out is FTIR and HPLC method. FTIR analysis carried out to determine of the compounds contained in the soga tingi bark extraction. Based on FTIR analysis it can be seen that there are O-H and N-H group in the wavenumber 3375,13 cm-1. C=O bond at wavenumber 1739,16 cm-1. C=C bond at wavenumber 1624,31 cm-1. C-H bond at wavenumbers 2970,72 cm-1, 1456,39 cm-1, and 1365,74 cm-1. NO2 bond at wavenumber 1365,74 cm-1. C-N bond at wavenumbers 1228,69 cm-1 and 1217,34 cm-1. And C-O bond at wavenumbers 1228,69 cm-1, 1217,34 cm-1, and 1052,3 cm-1. While HPLC analysis carried out to determine contains tannin level in the soga tingi bark extraction. HPLC conditions used are Flowrate: 1 mL/min, Mobile phase: MeOH : H2O (50:50), λ: 271 nm and Column: C18, 250 mm. Based on HPLC analysis it is known that the contains tannin level in the soga tingi bark extraction is 22,44 ppm.

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The identification and the quantitative determination of loratadine by the HPLC method

Žurnal organìčnoï ta farmacevtičnoï hìmìï ◽

10.24959/ophcj.21.240778 ◽

2021 ◽

Vol 19 (3(75)) ◽

pp. 40-46

Author(s):

Olena O. Mamina ◽

Volodymyr I. Kabachny ◽

Nataliia Yu. Bondarenko ◽

Olena V. Lozova

Keyword(s):

Quantitative Determination ◽

Mobile Phase ◽

Hplc Analysis ◽

Hplc Method ◽

Therapeutic Monitoring ◽

Reproducible Research ◽

Column Temperature ◽

Model Solutions ◽

Relative Standard

Aim. To develop the unified method of the HPLC analysis of loratadine, which can allow obtaining reliable and reproducible results of the studies of pharmaceuticals and biological matrices for monitoring the treatment effectiveness.Materials and methods. The HPLC analysis was performed on a “Milichrome A-02” microcolumn liquid chromatograph under the following conditions: a reversed-phase variant, 2 × 75 mm column filled with a non-polar sorbent Prontosil 120-5 C18 AQ, 5 μm; the mobile phase in the mode of a linear gradient – from eluent А (5 % of acetonitrile and 95 % of a buffer solution) to eluent B (100 % of acetonitrile) for 40 min. The flow rate of the mobile phase was 100 μL/min; the injection volume was 4 μL. The multichannel detection of the substance was carried out using an UV-detector at 210, 220, 230, 240, 250, 260, 280 and 300 nm; the optimal value of the column temperature was 37 – 40 °С, and the pump pressure was 2.8 – 3.2 MPa.Results and discussion. As a result of the studies performed, the retention parameters of loratadine and spectral relationships were determined using the unified HPLC method. This made it possible to include the results obtained in the database for the identification of antihistamines in the therapeutic monitoring of the treatment with an individual drug or in the complex treatment of allergic reactions. The development of the quantitative determination of loratadine by HPLC on model solutions using various concentrations of the drug was carried out. The content of loratadine was determined by the equation S = 1.14 × 10-3C – 0.50 × 10-4; the correlation coefficient was 0.9998. It was found that the relative standard deviation RSD did not exceed 0.93 % when analyzing loratadine in the model solutions by HPLC.Conclusions. The identification and the quantitative determination of loratadine by the unified HPLC method have been conducted. The method allows obtaining reliable and reproducible research results. The results of the studies can be recommended for implementation in the practice of forensic bureaus, toxicological centers, and clinical laboratories.

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Validation of A Simple HPLC-UV Method For the Quantification of Andrographolide in Self-Nano Emulsifying Drug Delivery System (Snedds) For Dissolution Study

International Journal of Drug Delivery Technology ◽

10.25258/ijddt.v7i04.10646 ◽

2017 ◽

Vol 7 (04) ◽

Author(s):

Syukri Y ◽

Afetma D. W. ◽

Sirin M. ◽

Fajri R. ◽

Ningrum A. D. K. ◽

...

Keyword(s):

Drug Delivery ◽

Drug Delivery System ◽

Delivery System ◽

Gastric Fluid ◽

Hplc Method ◽

Good Precision ◽

Intestinal Fluid ◽

Dissolution Medium ◽

Relative Standard ◽

Sufficient Precision

This research aim to validation of a simple, rapid and accurate HPLC-UV method for the quantification of andrographolide isolated from Andrographis paniculata Ness in Self Nano Emulsifying Drug Delivery System (SNEDDS) formulation during the dissolution test. The assay was performed using a XTerra® MS C18 column (150 mm X 4.6 mm, five μm) with a mobile phase of methanol and water (70: 30), at 0.8 mL/min flow rate and UV detection of 229 nm. Simulation gastric fluid (SGF) and intestinal fluid (SIF) were prepared as dissolution medium. The validation parameter was conducted including the test on linearity, precision, accuracy, LOD, and LOQ. The result showed an excellent linearity with r = 0.999 and good selectivity for both medium dissolution. The method showed sufficient precision, with a relative standard deviation (RSD) smaller than % Horwitz. The accuracy reported as % recovery was found to be 102.61 and 101.17 % in each SGF and SIF dissolution medium. LOD and LOQ were found 0.46 and 1.40 in SGF medium, 0.87 and 2.64 in SIF medium. In conclusion, the HPLC method developed showed specificity and selectivity with linearity in the working range, good precision and accuracy and suitable for quantification andrographolide in SNEDDS formulation.

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