scholarly journals Optimization and Validation of an HPLC-UV Method for Determination of Benzoic Acid and Sorbic Acid in Yogurt and Dried-Yogurt Products Using a Design of Experiment

2018 ◽  
Vol 18 (3) ◽  
pp. 522 ◽  
Author(s):  
Ala Yahya Sirhan
Keyword(s):  
Benzoic Acid ◽  
Design Of Experiment ◽  
High Performance ◽  
Sorbic Acid ◽  
Uv Detector ◽  
Column Temperature ◽  
Treatment Processes ◽  
Relative Standard ◽  
Pre Treatment ◽  
Solid Liquid

A method for the determination and analysis of benzoic acid and sorbic acid in yogurt and dried-yogurt products has been developed. This method was based on the use of a simple solid-liquid extraction method, followed by the high-performance liquid chromatography with a UV detector (HPLC–UV), enhanced with the aid of response surface methodology and design of experiment (DOE). The method excludes the use of complicated procedures, time-consuming and labor-intensive pre-treatment processes. Separation of the benzoic acid and sorbic acid with higher selectivity and sensitivity, and within reasonable retention time was performed by using an isocratic mobile phase of acetate buffer (pH 5.6)-methanol 60:40 at a column temperature of 25 °C. Optimization of sample preparation and analytical conditions gave recoveries in the range of 81 to 111% at spike levels of 2–20 mg/L and the relative standard deviations (RSDs) was lower than 9% in all cases. The intra-day precision and inter-day precision results were in the range of 8.4–8.5% and 10.4–11.0%. Additionally, the limits of detection (LOD) were 0.66 and 0.51 mg/L and the limits of quantification (LOQ) were 1.3 and 1.0 mg/L for benzoic acid and sorbic acid, respectively.

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).

ICH/FDA Guidelines-Compliant Validated Stability-Indicating HPLC-UV Method for the Determination of Axitinib in Bulk and Dosage Forms

2020 ◽  
Vol 16 (8) ◽  
pp. 1106-1112
Author(s):  
Ibrahim A. Darwish ◽  
Nasr Y. Khalil ◽  
Mohammad AlZeer
Keyword(s):  
High Performance ◽  
Kinase Inhibitor ◽  
Degradation Products ◽  
Internal Standard ◽  
Dosage Forms ◽  
Uv Detector ◽  
Stability Indicating ◽  
Therapeutic Benefits ◽  
Relative Standard

Background: Axitinib (AXT) is a member of the new generation of the kinase inhibitor indicated for the treatment of advanced renal cell carcinoma. Its therapeutic benefits depend on assuring the good-quality of its dosage forms in terms of content and stability of the pharmaceutically active ingredient. Objective: This study was devoted to the development of a simple, sensitive and accurate stabilityindicating high-performance liquid chromatographic method with ultraviolet detection (HPLC-UV) for the determination of AXT in its bulk and dosage forms. Methods: Waters HPLC system was used. The chromatographic separation of AXT, internal standard (olaparib), and degradation products were performed on the Nucleosil CN column (250 × 4.6 mm, 5 μm). The mobile phase consisted of water:acetonitrile:methanol (40:40:20, v/v/v) with a flow rate of 1 ml/min, and the UV detector was set at 225 nm. AXT was subjected to different accelerated stress conditions and the degradation products, when any, were completely resolved from the intact AXT. Results: The method was linear (r = 0.9998) in the concentration range of 5-50 μg/ml. The limits of detection and quantitation were 0.85 and 2.57 μg/ml, respectively. The accuracy of the method, measured as recovery, was in the range of 98.0-103.6% with relative standard deviations in the range of 0.06-3.43%. The results of stability testing revealed that AXT was mostly stable in neutral and oxidative conditions; however, it was unstable in alkaline and acidic conditions. The kinetics of degradation were studied, and the kinetic rate constants were determined. The proposed method was successfully applied for the determination of AXT in bulk drug and dosage forms. Conclusions: A stability-indicating HPLC-UV method was developed and validated for assessing AXT stability in its bulk and dosage forms. The method met the regulatory requirements of the International Conference on Harmonization (ICH) and the Food and Drug Administration (FDA). The results demonstrated that the method would have great value when applied in quality control and stability studies for AXT.

scholarly journals Analytical quality by design methodology for botanical raw material analysis: a case study of flavonoids in Genkwa Flos

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Min Kyoung Kim ◽  
Sang Cheol Park ◽  
Geonha Park ◽  
Eunjung Choi ◽  
Yura Ji ◽  
...  
Keyword(s):  
High Performance ◽  
Quality By Design ◽  
Analytical Data ◽  
Gradient Elution ◽  
Raw Material ◽  
Analytical Quality ◽  
Factor Screening ◽  
Column Temperature ◽  
Relative Standard ◽  
Critical Method

AbstractThe present study introduces a systematic approach using analytical quality by design (AQbD) methodology for the development of a qualified liquid chromatographic analytical method, which is a challenge in herbal medicinal products due to the intrinsic complex components of botanical sources. The ultra-high-performance liquid chromatography-photodiode array-mass spectrometry (UHPLC-PDA-MS) technique for 11 flavonoids in Genkwa Flos was utilized through the entire analytical processes, from the risk assessment study to the factor screening test, and finally in method optimization employing central composite design (CCD). In this approach, column temperature and mobile solvent slope were found to be critical method parameters (CMPs) and each of the eleven flavonoid peaks’ resolution values were used as critical method attributes (CMAs) through data mining conversion formulas. An optimum chromatographic method in the design space was calculated by mathematical and response surface methodology (RSM). The established chromatographic condition is as follows: acetonitrile and 0.1% formic acid gradient elution (0–13 min, 10–45%; 13–13.5 min, 45–100%; 13.5–14 min, 100–10%; 14–15 min, 10% acetonitrile), column temperature 28℃, detection wavelength 335 nm, and flow rate 0.35 mL/min using C18 (50 × 2.1 mm, 1.7 μm) column. A validation study was also performed successfully for apigenin 7-O-glucuronide, apigenin, and genkwanin. A few important validation results were as follows: linearity over 0.999 coefficient of correlation, detection limit of 2.87–22.41, quantitation limit of 8.70–67.92, relative standard deviation of precision less than 0.22%, and accuracy between 100.13 and 102.49% for apigenin, genkwanin, and apigenin 7-O-glucuronide. In conclusion, the present design-based approach provide a systematic platform that can be effectively applied to ensure pharmaceutically qualified analytical data from complex natural products based botanical drug.

scholarly journals HPLC-UV method for quantification of favipiravir in pharmaceutical formulations

2020 ◽  
Author(s):  
İbrahim Bulduk
Keyword(s):  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Potential Candidate ◽  
Column Temperature ◽  
Candidate Drug ◽  
System Suitability ◽  
Relative Standard

AbstractFavipiravir (FVP), a pyrazine analog, has shown antiviral activity against a wide variety of viruses. It is considered to be worth further investigation as a potential candidate drug for COVID-19. It is not officially available in any pharmacopoeia. A rapid, simple, precise, accurate, and isocratic high performance liquid chromatography (HPLC) method has been developed for routine quality control of favipiravir in pharmaceutical formulations. Separation was carried out by C18 column. The mobile phase was a mixture of 50 mM potassium dihydrogen phosphate (pH 2.3) and acetonitrile (90:10, v/v) at a flow rate of 1 mL min−1. The ultraviolet (UV) detection and column temperature were 323 nm, and 30 °C, respectively. The run time was 15 min under these chromatographic conditions. Excellent linear relationship between peak area and favipiravir concentration in the range of 10–100 μg mL−1 has been observed (r2, 0.9999). Developed method has been found to be sensitive (limits of detection and quantification were 1.20 μg mL−1 and 3.60 μg mL−1, respectively), precise (the interday and intraday relative standard deviation (RSD) values for peak area and retention time were less than 0.4 and 0.2%, respectively), accurate (recovery, 99.19–100.17%), specific and robust (% RSD were less than 1.00, for system suitability parameters). Proposed method has been successfully applied for quantification of favipiravir in pharmaceutical formulations.

scholarly journals DEVELOPMENT AND VALIDATION OF REVERSE PHASE-HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY TECHNIQUE FOR THE CONCOMITANT ASSESSMENT OF OMEPRAZOLE AND PIPERINE IN BULK FORM

2018 ◽  
Vol 11 ◽  
Author(s):  
Susithra E ◽  
Pavani Ch
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Correlation Coefficients ◽  
Literature Study ◽  
Uv Detector ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Relative Standard ◽  
Double Beam

Objective: The immense literature study was carried out and disclosed that here no method arrived for the concomitant assessment of omeprazole and piperine in bulk form by using RP-HPLC. Hence, an effort was assembled to arise a easy, specific, precise, reliable, linear, rapid, and validated reverse phase-high-performance liquid chromatography (RP-HPLC) technique for the simultaneous assessment of omeprazole and piperine in bulk form.Methods: The chromatographic analysis of omeprazole and piperine was performed using a RP-HPLC (WATERS) provided with autosampler and ultraviolet (UV) detector with the software of EMPOWER Version 2. The chosen conditions were isocratic separation with two mobile phase composed of acetonitrile:buffer (phosphate buffer: pH 6.5 ± 0.1) (55:45). Detection was carried out using UV/visible double-beam spectrophotometer at 320 nm. The method was validated as per the ICH guidelines.Results: The retention time for omeprazole and piperine by proposed HPLC method was found to be 2.767 and 4.029 min, respectively. The correlation coefficients are 0.999. The developed chromatographic method was found to be accurate with recovery 99.2–99.8% and was found within the acceptance criteria (i.e., 98.0–102.0%) with acceptable % relative standard deviation of not >2% at each level.Conclusion: Thus, the proposed HPLC procedure for the concomitant assessment of omeprazole and piperine was accurate, precise, linear, robust, simple, and economic. 

Determination of Trace Level Oxytetracycline and Influences of Coexisting Pollutants on its Sorption by Three Kinds of Sludge

2011 ◽  
Vol 383-390 ◽  
pp. 862-865
Author(s):  
Man Hong Huang ◽  
Liang Chen ◽  
Dong Hui Chen ◽  
Yu Dong Yang
Keyword(s):  
High Performance ◽  
Anaerobic Sludge ◽  
Sorption Behavior ◽  
Wastewater Sample ◽  
Uv Detector ◽  
Linear Calibration ◽  
Trace Level ◽  
Relative Standard ◽  
Strong Anion Exchange ◽  
Oasis Hlb

Strong anion exchange (SAX) columns and oasis HLB cartridges were combined to extract trace level oxytetracycline(OTC) and high performance liquid chromatography(HPLC) UV-detector were used to measure it in wastewater sample. The effect of mobile phase was investigated. Under the best analysis conditions, linear calibration equations were established for OTC. The linearity were in the range of 0.1-10g/mL, Correlation coefficient (R2) is about 0.9997. The recovery factors ranged from 82-92% with a relative standard deviation of 4.8-6.4%.Lab-scale experiments were conducted to investigate the sorption behavior of OTC by anaerobic sludge. Starch in the mixed liquor can decrease the adsorption capacity of OTC.

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.

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