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

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).

Author(s):  
Susithra E ◽  
Pavani Ch

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. 


2020 ◽  
Vol 11 (1) ◽  
pp. 311-314
Author(s):  
Gulnara G. Galyautdinova ◽  
Vladislav I. Egorov ◽  
Alexander M. Saifutdinov ◽  
Elvira R. Rakhmetova ◽  
Andrey V. Malanev ◽  
...  

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.


2010 ◽  
Vol 7 (3) ◽  
pp. 962-966 ◽  
Author(s):  
Naveen Kumar ◽  
Nishant Verma ◽  
Omveer Songh ◽  
Naveen Joshi ◽  
Kanwar Gaurav Singh

A simple, precise, sensitive, fast and accurate high performance liquid chromatography method has been developed for the determination of atenolol using mixture of phosphate buffer and acetonitrile (53:47 v/v) as mobile phase. Buffer was prepared by mixing 0.02 M K2PO4and 0.003 M KH2PO4in equal proportion. Detection was carried out using UV detector at λmax230 nm. Column was ODS and dimensions of column was 25 mm × 4.6 mm. Atenolol was eluted out at retention time of 2.1 min. Method was validated at 1.2 mL/min flow rate. Calibration curve was linear between ranges of 40 to 200 mcg concentration. The limit of detection was calculates 120 nano gram and limit of quantitation is 510 nano gram. The relative standard deviation (RSD) of atenolol was 0.6. The percentage recovery of atenolol was 99.6%.


2021 ◽  
Vol 5 (4) ◽  
pp. 353-358
Author(s):  
Wiwin Winingsih ◽  
Sri Gustini Husein ◽  
Rozalia Putri Neno Ramdhani

Ethyl para-methoxycinamate (EPMS) is a major compound of Kaempferia galanga L that has anti-inflammatory effect.  The purpose of this study was to determine of EPMS in Kaempferiae galanga L rhizome extract by  High Performance Liquid Chromatography (HPLC) and evaluated the performance of the analysis. This study included determination of system suitability, accuracy, precision, linearity and range, limit of detection (LOD) and Limit of quantitation (LOQ) and selectivity.  The results of system suitability test  HPLC System for EPMS analysis were as follows isocratic elution system of a mobile phase mixture of methanol: water (70:30) containing 0.1% TFA, uv detector at a wavelength of 308 nm using column C18 (150 × 4, 6mm, 5μm) flow rate 1 ml / min. From the analysis, it was found that the average EPMS content was 78.74%. Then method had linear concentration range from 5-360 ppm, with R ² = 0.9999. The LOD and LOQ were 7.0722 ppm and 21.4311 ppm respectively. The accuracy of this method that represented by % recovery was 98.02% - 101.26%. The precision of this method that expressed by Relative Standard Deviation (RSD) was 1.57%. The selectivity of this method that showed by  resolution value was 2.6. Based on the results of the system suitability test and analysis performance evaluation,all parameters met the requirements.


2020 ◽  
Vol 17 ◽  
Author(s):  
Lei Zheng ◽  
Jing Yang ◽  
Yu-yao Guan ◽  
Lei Zhang ◽  
Chao Song ◽  
...  

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.


2021 ◽  
Vol 13 (13) ◽  
pp. 6998
Author(s):  
Beibei Qi ◽  
Chao Wu ◽  
Huiling Liang ◽  
Kehui Cui ◽  
Shah Fahad ◽  
...  

Liquid-liquid extraction and solid phase extraction followed by high-performance liquid chromatography (HPLC) connected with ultraviolet (UV) detection were used for the determination of phytohormones. The parameters influencing the performance of the HPLC-UV method, including composition of the mobile phase for gradient elution, column temperature, flow rate, and detection wavelength, were optimized. This method can simultaneously determine 11 phytohormones, including nine cytokinins, indole-3-acetic acid, and abscisic acid. The limit of detection of this method is 0.22 to 1.1 µg L−1, and the coefficient factors of linear regression are >0.998. The recoveries of the target phytohormones ranged between 62.1~109.4%, and the relative standard deviations were <10%. This method is suitable for determining phytohormones, especially cytokinins, in young panicles, roots, and xylem sap of rice plants.


2016 ◽  
Vol 11 (1) ◽  
pp. 38
Author(s):  
Liliek Nurhidayati ◽  
Siti Sofiah ◽  
Ros Sumarny ◽  
Kevin Caesar

<p>Mangosteen fruit rind extract contain a lot of antioxidants. α-Mangostin is a component in mangosteen fruit rind that has highest antioxidant effect. The oral solution containing mangosteen fruit rind extract is required an assay method for quality assessment. Determination of a very low concentration of analyte in sample with very complex matrix, such as α-mangostin in oral solution, needs a selective and sensitive method, such as high performance liquid chromatography (HPLC). In this study, α-mangostin assay was performed by reverse phase HPLC system using octadecylsilane (C18) as stationary phase,  methanol-water (90:10) as mobile phase, the flow rate is 1.0 mL/min, and the UV detector at 316 nm. The retention time of α-mangostin was 9.622 minutes. Peak of α-mangostin was well separated with resolution of 1.725. Linearity was in the range of 1.67-5.01 ppm with correlation coefficient of 0.9986. The relative standard deviation (RSD) was 1.30 %, the recovery was in the range of 95.80-100.76 </p>


2015 ◽  
Vol 11 (1) ◽  
pp. 38
Author(s):  
Liliek Nurhidayati ◽  
Siti Sofiah ◽  
Ros Sumarny ◽  
Kevin Caesar

<p>Mangosteen fruit rind extract contain a lot of antioxidants. α-Mangostin is a component in mangosteen fruit rind that has highest antioxidant effect. The oral solution containing mangosteen fruit rind extract is required an assay method for quality assessment. Determination of a very low concentration of analyte in sample with very complex matrix, such as α-mangostin in oral solution, needs a selective and sensitive method, such as high performance liquid chromatography (HPLC). In this study, α-mangostin assay was performed by reverse phase HPLC system using octadecylsilane (C18) as stationary phase,  methanol-water (90:10) as mobile phase, the flow rate is 1.0 mL/min, and the UV detector at 316 nm. The retention time of α-mangostin was 9.622 minutes. Peak of α-mangostin was well separated with resolution of 1.725. Linearity was in the range of 1.67-5.01 ppm with correlation coefficient of 0.9986. The relative standard deviation (RSD) was 1.30 %, the recovery was in the range of 95.80-100.76 </p>


2021 ◽  
Vol 12 (3) ◽  
pp. 1709-1717
Author(s):  
Haritha G ◽  
Vijey Aanandhi M ◽  
Shanmugasundaram P

This study explains about the Analytical Quality by Design approach for the optimization of a High-Performance Liquid Chromatography Method for the simultaneous estimation of Metformin and Ertugliflozin in pharmaceutical substance. The study aimed to optimize the High-Performance Liquid Chromatography (HPLC) by means of an analytical target profile in order to achieve good separation of compounds along with acceptable analysis time. Identification of risk factors for variables affects the method efficacy. This leads to the development of an accurate, precise, and economic method. The optimized conditions of the developed method were a stationary phase of a Discovery C18 250 x 4.6mm, 5m and a mobile phase of Orthophosphoric acid buffer (pH 2.2),ACN taken in the ratio 60:40 was selected as mobile phase and detection wavelength of 230nm. The flow rate was selected as 0.98ml/min at 29.150C column temperature. Using the central composite design (CCD) method was optimized. The method is showing the linearity over the concentration range of 25-150µg/ml for Metformin and 0.375-2.25µg/ml for Ertugliflozin. The intra-and inter-day precision were less than 2% of relative standard deviation. Accuracies between  99-102% of the true values.The LOD obtained for Metformin and Ertugliflozin were found to be 59 and 3.7, respectively.  LOQ obtained for Metformin and Ertugliflozin were 77.6 and 5.2, respectively.Under accelerated conditionsdegradation percentage of the drug was found to be less than 10%, and the degradation product peak not affecting the system suitability of Metformin and Ertugliflozin.


Author(s):  
Lenche Velkoska-Markovska ◽  
Biljana Petanovska-Ilievska

AbstractThe quality of pesticide formulations has an impact on the crop safety, environment and human health. Therefore, the development of new analytical methods for the determination of active substances in pesticide formulations in order to control their quality, as well as, their residues in food samples in order to ensure food safety, is always welcome. A new, simple, precise and accurate normal-phase high-performance liquid chromatography (NP-HPLC) method for determination of an active ingredient malathion in the commercial emulsifiable concentrate pesticide product has been developed and validated. The analysis was carried out on a LiChrosorb CN (250 x 4 mm, 5 μm) analytical column using isocratic elution with mobile phase consisted of n-hexane and dichloromethane (80/20, v/v), flow rate of 1 mL/min, constant column temperature at 25 °C and ultraviolet diode-array detection at 220 nm. The obtained values for multiple correlation coefficients (R2 ≥ 0.9990), relative standard deviation of retention times, peak areas and heights (RSD ≤ 1.14%), recoveries ranged from 98.97 to 101.62%, revealed that the developed method has a satisfactory linearity, precision and accuracy. Also, the developed method was successfully applied for determination of malathion residues in apple juice samples, after preliminary sample preparation using solid-phase extraction. Specificity, selectivity, linearity, matrix effect, precision and accuracy were tested in order to validation of this method. The obtained results were in acceptable ranges and indicated that the developed method is suitable for routine determination of malathion in the pesticide formulation, as well as for determination of malathion residues in apple juice samples. The run time of HPLC analysis was about 6 min.


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