scholarly journals Detection of tetracycline antibiotics in honey using high-performance liquid chromatography

2020 ◽  
Vol 11 (1) ◽  
pp. 311-314
Author(s):  
Gulnara G. Galyautdinova ◽  
Vladislav I. Egorov ◽  
Alexander M. Saifutdinov ◽  
Elvira R. Rakhmetova ◽  
Andrey V. Malanev ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Honey Bee ◽  
High Performance ◽  
Hplc Method ◽  
Tetracycline Hydrochloride ◽  
Uv Detector ◽  
Column Temperature ◽  
Tetracycline Antibiotics ◽  
Safety Control

It is hard to overestimate the value of honey since the constituent substances in it are of great importance in the food industry and medicine. The quality of honey is established by the legislation of the Russian Federation (GOST). But the levels of these standards are regulated by outdated methods of analysis, which can not give reliable results. The detection of antibiotic residues in honey is a central issue in the quality and safety control of this product. Accumulation of drugs in honey used to treat bee colonies can cause allergies and dysbiosis in people who have eaten such honey, as well as develop antibiotic resistance in microorganisms. At present, one of the promising directions in the field of detecting medicines in honey is the use of high-performance liquid chromatography (HPLC). It helps selectively and accurately detect antibiotic substances in honey bee products. In Russia, the HPLC method is used with mass spectrometry to detect tetracycline residues in honey. A significant drawback with this method that limits the widespread use of it is the application of expensive, technically sophisticated equipment that needs high-quality reagents and consumables. The purpose of this work was to develop the simultaneous identification of tetracycline antibiotics in honey and carry out their quantitative analysis by a reversed-phase HPLC method. A sample preparation algorithm was developed, and the conditions for chromatographing combined indication of tetracyclines in honey at an acceptable concentration according to the MRL (0.01 mg/kg) with Agilent 1260 Infiniti liquid chromatograph equipped with a column thermostat, a gradient pump, and a UV detector were selected. According to the results of the research, the most optimal condition for the simultaneous analysis of oxytetracycline, tetracycline hydrochloride, chlortetracycline in honey by HPLC method with ultraviolet detection was a wavelength of 254 nm, a flow rate of 0.5 ml/min and a column temperature of 25° C. Under these conditions, the antibiotic retention time was determined: 4.069 minutes for oxytetracycline, 4.331 minutes for tetracycline hydrochloride, 4.642 minutes for chlortetracycline. The developed HPLC method for the simultaneous determination of tetracycline antibiotics in honey was tested on honey bee products from the regions of the Republics of Tatarstan and Bashkortostan.

scholarly journals A SIMULTANEOUS ESTIMATION, VALIDATION AND FORCED DEGRADATION STUDIES OF 5-FLUOROURACIL AND TEGAFUR IN A PHARMACEUTICAL DOSAGE FORM USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD

2018 ◽  
Vol 11 (12) ◽  
pp. 132
Author(s):  
Vaishali Mistry ◽  
Akshay Yelwe ◽  
Amey Deshpande
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Stability Indicating ◽  
Rp Hplc ◽  
The Stability

Objective: The present study describes the stability indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of 5-fluorouracil and tegafur in pharmaceutical dosage forms.Method: 5-fluorouracil and tegafur the propose RP-HPLC method were developed by using Shimadzu Prominence-i LC-2030 HPLC system equipped with UV detector and chromatographic separation was carried on shim-pack gist c18 (250 × 4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the run time was 10 min. The mobile phase consisted of methanol and water in the ratio of 50:50% v/v and elements were scanned using a UV detector at 271 nm.Result: The retention time of 5-fluorouracil and tegafur was found to be 2.74 and 3.66 min, respectively. A linearity response was observed in the concentration range of 13.4 μg/ml–31.3 μg/ml for 5-fluorouracil and 6 μg/ml–14 μg/ml for tegafur, respectively. Limit of detection and limit of quantification of 5-fluorouracil were 10.97 μg/ml and 33.26 μg/ml and for tegafur are 4.89 μg/ml and 14.83 μg/ml, respectively.Conclusion: The stability indicating that the method was developed by subjecting drugs to stress conditions such as acid and base hydrolysis, oxidation, photo and thermal degradation, and degraded products formed were resolved successfully from samples.

Analysis of Bifenthrin and its Enantiomer Using High Performance Liquid Chromatography

2014 ◽  
Vol 675-677 ◽  
pp. 275-279 ◽  
Author(s):  
Su Su Fan ◽  
Jian Shi ◽  
Ling Zhou ◽  
Yu Wen Hang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Chiral Stationary Phase ◽  
Ammonium Acetate ◽  
Hplc Method ◽  
Column Temperature ◽  
Polysaccharide Derivatives ◽  
Separation Results

Using the high performance liquid chromatography (HPLC) method, bifenthrin isomers can be split at a polysaccharide derivatives chiral stationary phase column, and two well distinguished peaks of bifenthrin isomers are obtained. The effects of mobile phase ratios, temperatures, and detection wavelengths on the separation results are discussed. The optimal chromatographic conditions are as follows: the mobile phase ratio is methanol: ammonium acetate salts = 80:20, the column temperature is 35°C, and the wavelength is set as 220 nm. Under the optimal conditions, the resolution of bifenthrin enantiomer can be as large as 3.0.

scholarly journals Determination of Ketotifen Fumarate in Syrup Dosage Form by High Performance Liquid Chromatography

2020 ◽  
pp. 63-72
Author(s):  
Mohammed Ali Salih ◽  
Dlivan Fattah Aziz ◽  
Salar Ibrahim Ali
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Column Temperature ◽  
Ketotifen Fumarate ◽  
Suggested Technique ◽  
Elution Method

The goal of the current study was to establish and authenticate an isocratic reverse-stage High-Performance Liquid Chromatography (HPLC) method for quantifying ketotifen fumarate (KF) in pharmaceutical liquid dosage compositions. Easy, quick, accurate, exact, and accurate reverse-stage high-performance liquid chromatography was advanced for the simultaneous assessment of ketotifen fumarate in the liquid syrup dosage type. The HPLC system using isocratic elution method with reverse-phase Inertsil ODS-(250 mm × 4.6 mm, 3 μm) column was detected by ultraviolet absorbance at 297 nm with no interference from widely using excipients, the mobile phase (A) is a mixture of triethylamine and water (175 μl in 500 ml of water), and the mobile phase (B) is a mixture of triethylamine and methanol (175 μl in 500 ml of methanol) at a flow rate of 1.5 mL/min (mobile phase A 40 %:mobile phase B 60%) at column temperature using 40 ° C, the retention time for ketotifen fumarate was 6.4±0.5 min. The concentration curves were linear in the range of 10.0 to 35.0 μg / ml (R2 = 0.9999). The developed method was tested for the specificity, precision, linearity, precision, reliability, robustness, and consistency of the solution. The regeneration of ketotifen fumarate in formulations was found to be 99.75 %, 99.91 %, and 100.05 % respectively. The percent RSD for percent recovery was found to be 0.21 and 0.17 and 0.10 for ketotifen fumarate. In the conclusion, the suggested technique was successfully used for the quantitative determination of ketotifen fumarate in formulations.

Chiral Resolution and Content Determination of Ketorolac Tromethamine Using High-performance Liquid Chromatography

2020 ◽  
Vol 17 ◽  
Author(s):  
Lei Zheng ◽  
Jing Yang ◽  
Yu-yao Guan ◽  
Lei Zhang ◽  
Chao Song ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Chiral Resolution ◽  
Ketorolac Tromethamine ◽  
Column Temperature ◽  
Relative Standard ◽  
Determination Methods

Background:: Establishing R, S-enantiomer (S-KT and R-KT) chiral resolution and determination methods for KT are of great significance. Objective:: This study aimed to establish a high-performance liquid chromatography (HPLC) method for the resolution and determination of ketorolac tromethamine (KT) enantiomers. Methods:: A CHIRALPAK AGP column (0.4  10 cm, 5 μm) was used with 10 mmol/L ammonium acetate (pH 5.5) and isopropanol (97:3) as the mobile phase. The detection wavelength was 324 nm, the flow rate was 1.0 mL/min, the column temperature was 25°C, and the injection volume was 5 μL. Results:: The resolution between S-KT and R-KT was 2.8. S-KT and R-KT demonstrated a good linear relationship in the range of 3-60 μg/mL (r > 0.999). The average recoveries of S-KT and R-KT were 99.2% and 99.8%, with relative standard deviations of 2.0% and 2.4%, respectively. Conclusion:: The established method can be used for the resolution and determination of S-KT and R-KT.

scholarly journals METHOD DEVELOPMENT AND FORCE DEGRADATION STUDIES FOR SIMULTANEOUS ESTIMATION OF SALBUTAMOL SULFATE, ETOFYLLINE AND BROMHEXINE HYDROCHLORIDE IN PHARMACEUTICAL DOSAGE FORM USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD

2018 ◽  
Vol 11 (8) ◽  
pp. 378 ◽  
Author(s):  
Nutan Rao ◽  
Kajal D Gawde
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Salbutamol Sulfate ◽  
Uv Detector ◽  
Rp Hplc ◽  
The Stability

Objective: The present study describes the stability indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of salbutamol sulfate (SAL), etofylline (ETO), and bromhexine hydrochloride (BROM) in pharmaceutical dosage forms.Methods: The proposed RP-HPLC method was developed using Shimadzu prominence-i LC-2030 HPLC system equipped with ultraviolet (UV) detector and chromatographic separation was achieved isocratically using Shim-pack C18 (250 mm×4.6mm, 5 μ) column at a flow rate of 1 ml/min and the run time was 13 min. The mobile phase consisted of acetonitrile: 0.1M potassium dihydrogen phosphate buffer (35:65) with pH adjusted to 3.0 and eluents were scanned using UV detector at 225 nm.Result: The retention time of SAL, ETO, and BROM was found to be 2.319 min, 2.698 min, and 10.329 min, respectively. The calibration curve was linear over the concentration ranges of 1.6–3.2 μg/ml, 160–320 μg/ml, and 6.4–12.8 μg/ml for SAL, ETO, and BROM, respectively.Conclusion: The stability indicating method was developed by subjecting the drugs to stress conditions such as acid and base hydrolysis, oxidation, humidity, and photo- and thermal degradation and the degraded products formed were resolved successfully from the samples. Therefore, the proposed method can be used as a more convenient and efficient option for the simultaneous estimation of all the three drugs in bulk and combined

scholarly journals SIMULTANEOUS ESTIMATION AND FORCED DEGRADATION STUDIES OF AMILORIDE HYDROCHLORIDE AND FUROSEMIDE IN A PHARMACEUTICAL DOSAGE FORM USING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD

2018 ◽  
Vol 11 (7) ◽  
pp. 215 ◽  
Author(s):  
Javed S Shaik ◽  
Nutan N Rao
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Reverse Phase ◽  
Rp Hplc ◽  
The Stability ◽  
Amiloride Hydrochloride

Objective: The present study describes the stability indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of amiloride hydrochloride and furosemide in pharmaceutical dosage forms.Methods: The proposed RP-HPLC method was developed using Shimadzu LC-2030 HPLC system equipped with UV detector, and chromatographic separation was carried on Shim-pack C18 (250 mm×4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the runtime was 4min. The mobile phase consisted of water and acetonitrile in the ratio of 35:65, and elements were scanned using a UV detector at 281 nm.Results: The retention time of amiloride hydrochloride and furosemide was found to be 1.92 min and 3.14min, respectively. Linearity was found to be 12–28 ppm for amiloride hydrochloride and 96–224 ppm for furosemide, respectively. Limit of detection and limit of quantification for amiloride hydrochloride were 0.381 ppm and 1.156 ppm and for furosemide were 2.00 ppm and 6.068 ppm, respectively.Conclusion: The stability indicating method was developed by subjecting the drugs to stress conditions such as acid and base hydrolysis, oxidation, humidity, photolytic, and thermal degradation, and the degraded products formed were resolved successfully from the samples.

scholarly journals Determination of Caffeic Acid in Ethanolic Extract of Spent Coffee Grounds by High-Performance Liquid Chromatography with UV Detection

2021 ◽  
Vol 21 (5) ◽  
pp. 1281
Author(s):  
Michael Raharja Gani ◽  
Enade Perdana Istyastono
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Caffeic Acid ◽  
High Performance ◽  
Spent Coffee Grounds ◽  
Uv Detector ◽  
Column Temperature ◽  
Coffee Grounds ◽  
Spent Coffee Ground ◽  
Relative Standard

We developed a method for determining the caffeic acid in spent coffee grounds. The spent coffee ground solution was prepared by blending 3 g spent coffee grounds with 60 mL ethanol/water (40/60 v/v) for 2 h on a hot plate magnetic stirrer (60 °C, 350 rpm). The mixture was filtered and the filtrate was concentrated under vacuum (60 °C) to 5 mL. The method employed a reversed-phase high-performance liquid chromatography with a UV detector. We used a Phenomenex Luna column (250 × 4.6 mm; i.d., 5 µm) under isocratic elution, and the mobile phase was acetonitrile-methanol-aqueous formic acid (10:10:80 v/v), with a flow rate of 0.9 mL/min. Analysis was performed at 324 nm. The column temperature was set at 27 °C temperature. The results showed that this method was selective for quantifying the caffeic acid in spent coffee grounds with good linearity in the range of 1.31–17.07 μg/mL. The detection and quantitation limits were 0.28 and 0.84 μg/mL, respectively. The mean intraday and interday recoveries were 83.80–95.17% and 82.16–97.40%, respectively. Intraday and interday precision expressed as the relative standard deviation (RSD) were below 7.3%. There was 0.17% ± 0.006 w/w caffeic acid in the spent coffee grounds (RSD = 3.63%, n = 3).

Establishment and Evaluation of Determination of Cinnamaldehyde in Baoyuanqingxue Granules by HPLC

2014 ◽  
Vol 998-999 ◽  
pp. 372-377 ◽  
Author(s):  
Qiang Wu ◽  
Chang Hong Wang ◽  
Pu Wang ◽  
Xiang Rong Liu
Keyword(s):  
Quality Control ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Extraction Method ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Column Temperature ◽  
Average Recovery

To examine the extraction method and chromatographic conditions that affect the determination of cinnamaldehyde in Baoyuanqingxue granules and make clinical evaluation about the determination of cinnamaldehyde.Ultrasonic methanol extraction was used before the detemination of cinnamaldehyde in Baoyuanqingxue granules. High Performance Liquid chromatography (HPLC) method was applied to detect samples. The SB-C18 column (Agilent, ZORBAX, 4.6×150mm, 5μm) was adopted, the mobile phase was acetonitrile-water (35:65) at the flow rate of 1.00mL•min-1 with DAD detection wavelength at 290nm, the volume of injection was 20μL and the column temperature was 30°C. The resolution between cinnamaldehyde and other peaks was good. The calibration curve was linear in the range of 0.5035~50.35μg•mL-1(r=0.99976). The average recovery (n=6) of cinnamaldehyde was 99.2% with RSD of 0.5%. The HPLC-DAD method to detect the content of cinnamaldehyde in Baoyuanqingxue granules is simple and accurate. It can be used for quality control of cinnamaldehyde in Baoyuanqingxue granules.

Colorimetry and High Performance Liquid Chromatography of Atrazine Residues in Soil: Comparison of Methods

1980 ◽  
Vol 63 (3) ◽  
pp. 506-510
Author(s):  
Thomas M Vickrey ◽  
Dori L Karlesky ◽  
Gary L Blackmer
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Methylene Chloride ◽  
Colorimetric Method ◽  
Hplc Method ◽  
Full Scale ◽  
Uv Detector ◽  
Reaction Solution ◽  
Full Scale Deflection

Abstract The colorimetric method for determining residual atrazine levels in soil is compared with reverse phase high performance liquid chromatography (HPLC). The soil samples are extracted with water-acetonitrile (10 + 90) and the filtrate is partitioned with methylene chloride. For the colorimetric analysis the organic phase is filtered through activity V alumina, collected, and evaporated to dryness. The residue is dissolved first in ethyl ether, and then in water as the ether is removed. The atrazine solution is buffered (citric acid, pH 7.0) and heated with added pyridine. When the reaction is complete, the product is complexed with ethylcyanoacetate, and the solution absorbance is measured at 550 nm. The complex obeys Beer’s law and has a sensitivity of 230 ng for a 1% full scale deflection at 1 AUFS. For the HPLC method, the methylene chloride extract is dried, the chromatographic solvent is quantitatively added (either chloroform or methanol), and the solution is analyzed with a UV detector at 254 nm. Minimum amount detectable for a 1% full scale deflection is 5 ng at 0.01 AUFS. Soil background interferences were investigated for both methods, and buffering the pyridine-triazine reaction solution was the most efficient method for removing the background for colorimetry. The recovery efficiencies for the colorimetric and HPLC methods were 45.5 ± 3.8% and 94.4 ± 3.4%, respectively.

scholarly journals Development of a high performance liquid chromatography method for simultaneous analysis of theophylline, guaifenesin and diphenhydramine in an elixir

2017 ◽  
Vol 16 (10) ◽  
pp. 2501-2506 ◽  
Author(s):  
Yahdiana Harahap Hayun ◽  
Maria O. Puspasari
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Low Cost ◽  
Hplc Method ◽  
Simultaneous Analysis ◽  
Uv Detector ◽  
Chromatography Method ◽  
Mobile Phase Flow Rate ◽  
Diphenhydramine Hydrochloride

Purpose: To develop and validate a new low-cost high performance liquid  chromatography (HPLC) method for simultaneous analysis of theophylline (TH), guaifenesin (GF) and diphenhydramine hydrochloride (DH) in elixir dosage form.Methods: Chromatographic conditions were an isocratic elution with C18-Kromasil® column (250 x 4.6 mm, 5 μm), methanol-water (1:1, v/v, pH 3,0) as mobile phase, flow rate 1.0 ml/min and UV detector at λ 218 nm. The method was validated for selectivity, linearity, LOD-LOQ, precision, and accuracy.Results: Retention time of TH, GF and DH was 3.3, 5.3 and 9.1 min, respectively. The method showed good selectivity, calibration curves were linear over the concentration range of 1.000 – 10.002 μg/mL, 0.801 – 8.008 μg/mL, and 0.251 – 2.514 μg/mL (r2 > 0.999). LOD was 0.1093, 0.16520, and 0.0706 μg/mL, while LOQ was 0.3645, 0.5506, and 0.2354 μg/mL for TH, GF and DH, respectively. Recovery accuracy was 99.77 - 101.10, 100.50 - 101.95 and 99.20 - 100.13 % for TH, GF and DH, respectively; precision (RSD) was < 2.0.Conclusion: The proposed method is highly selective, sensitive, precise, and  accurate, and would suitable for the simultaneous analysis of TH, GF, and DH in elixir dosage form. Since methanol is cheaper than acetonitrile, the application of the method may reduce the cost of analysis.Keywords: Simultaneous analysis, Theophylline, Guaifenesin, Diphenhydramine hydrochloride, Elixir

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