scholarly journals Analysis of gallic acid and ellagic acid in leaves of Elaeagnus angustifolia L. from different habitats and times in Xinjiang by HPLC with cluster analysis

2020 ◽  
Author(s):  
Yun Sun ◽  
Jiajia Liu ◽  
Shasha Tang ◽  
Xiaoying Zhou ◽  
Keyword(s):  
Gallic Acid ◽  
Correlation Coefficient ◽  
Ellagic Acid ◽  
High Performance ◽  
Hierarchical Cluster ◽  
Gradient Elution ◽  
Chromatographic Column ◽  
Elaeagnus Angustifolia ◽  
R Software ◽  
Relative Standard

AbstractObjectiveTo determine the levels of gallic acid and ellagic acid by using high-performance liquid chromatography (HPLC) with R software hierarchical cluster analysisin Elaeagnus angustifolia L. gathered from different locations in Xinjiang.MethodsA chromatographic column Diamonsil C18 with a size of 4.6 × 250 mm and 5 μm was used with methanol as A and 0.1% phosphoric acid aqueous solution as B as the mobile phase. The flow rate was 1 mL/min for the gradient elution and the injection volume was 5 μL. HPLC was performed with a detection wavelength of 260 nm and chromatographic column of 35 °C. In addition, R software hierarchical clustering method was used for studying the levels of gallic acid and ellagic acid in E. angustifolia L. from 10 areas.ResultsGallic acid and ellagic acid showed a good linear relationship between 7.375 and 236 μg/mL with a correlation coefficient of 0.9999, and between 3.625 and 116 μg/mL with a correlation coefficient of 0.9999 respectively. The average recovery values were 103.98 and 101.57%, and the Relative Standard Deviation (RSD) values were 1.92 and 1.47%.ConclusionDifferences in the levels of gallic acid and ellagic acid in E. angustifolia L. leaves from different areas in Xinjiang showed that both were the highest in Kuitun.

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.

Validation of HPLC Method for Determination of Histamine in Human Immunoglobulin Formulations

2020 ◽  
Vol 103 (5) ◽  
pp. 1223-1229
Author(s):  
Michikazu Tanio ◽  
Toru Nakamura ◽  
Hideki Kusunoki ◽  
Kyohei Ideguchi ◽  
Kazuyuki Nakashima ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
High Performance ◽  
Gradient Elution ◽  
Hplc Method ◽  
Human Immunoglobulin ◽  
Histamine Dihydrochloride ◽  
Relative Standard

Abstract Background Histamine fixed-immunoglobulin formulations, which consisted of 0.15 µg of histamine dihydrochloride and 12 mg of human immunoglobulin in a vial, are used for anti-allergic treatments, and controlling the amounts of histamine in the formulations is essential to avoid histamine intoxication. Objective A high-performance liquid chromatography (HPLC) method for determination of histamine contents of the formulations was established and validated. Methods Histamine extracted from the formulation was labeled with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate and was analyzed by gradient elution HPLC with UV detection at 260 nm. Results The method showed linearity in the range 0.8–2.4 µM (R > 0.999), accuracy (100.1–105.8% recovery), and precision (relative standard deviation ≤ 1.93%). The validated method was applied for five lots of the pharmaceutical, and their histamine contents were determined to be 0.149–0.155 µg/vial. Conclusions These results indicated that the validated method is useful to control amounts of histamine in biopharmaceutical products. Highlights The HPLC method was developed for quantitative determination of histamine content of the histamine fixed-immunoglobulin formulations.

scholarly journals High-Performance Thin-Layer Chromatography Densitometric Method for Simultaneous Quantitation of Phyllanthin, Hypophyllanthin, Gallic Acid, and Ellagic Acid in Phyllanthus amarus

2006 ◽  
Vol 89 (3) ◽  
pp. 619-623 ◽  
Author(s):  
Kamlesh Dhalwal ◽  
Yogesh S Biradar ◽  
Mandapati Rajani
Keyword(s):  
Thin Layer ◽  
Gallic Acid ◽  
Thin Layer Chromatography ◽  
Ellagic Acid ◽  
High Performance ◽  
Raw Material ◽  
Phyllanthus Amarus ◽  
Whole Plant ◽  
Recovery Study ◽  
Layer Chromatography

Abstract Whole plant of Phyllanthus amarus Linn. is a reputed drug of the Indian systems of medicine that is used as hepatoprotective agent. A simple high-performance thin-layer chromatography (HPTLC) densitometric method has been developed for the simultaneous quantitation of phyllanthin, hypophyllanthin, gallic acid, and ellagic acid in the whole plant of P. amarus. They were found at levels of 0.37, 1.16, 0.36, and 0.17% (w/w), respectively. The method was validated for precision, repeatability, and accuracy. Instrumental precision was found to be 0.54, 0.93, 0.08, and 0.78% (coefficient of variation, CV); repeatability of the method was 1.01, 0.79, 0.98, and 1.06% (CV) for phyllanthin, hypophyllanthin, gallic acid, and ellagic acid, respectively. Accuracy of the method was determined by a recovery study conducted at 3 different levels, and the average recovery was found to be 99.09% for phyllanthin, 99.27% for hypophyllanthin, 98.69% for gallic acid, and 100.49% for ellagic acid. The proposed HPTLC method was found to be simple, precise, specific, sensitive, and accurate and can be used for routine quality control of raw material of P. amarus and formulations containing P. amarus. It also has the applicability in quantitating any of these marker compounds in other drugs.

scholarly journals A NOVEL REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS ESTIMATION OF ELLAGIC ACID, QUERCETIN, AND PIPERINE IN AYURVEDIC FORMULATIONS

2018 ◽  
Vol 11 (6) ◽  
pp. 312
Author(s):  
Sultana Shaikh ◽  
Vandana Jain
Keyword(s):  
Ellagic Acid ◽  
High Performance ◽  
Quantitative Estimation ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Column Temperature ◽  
Relative Standard ◽  
Liquid Chromatographic

Objective: The objective of the study was to develop a novel, accurate, precise, and linear reverse-phase high-performance liquid chromatographic (RP-HPLC) method for simultaneous qualitative and quantitative estimation of ellagic acid, quercetin, and piperine in different Ayurvedic formulations and validate as per the International Conference on Harmonization guidelines. Methods: In the present work, a good chromatographic separation was achieved isocratically using a shim-pack HPLC C18 column (4.6×250 mm, 5 μm) and a mobile phase consisting of 0.02 M potassium dihydrogen orthophosphate buffer (pH adjusted to 3.5 with orthophosphoric acid) and acetonitrile in the ratio 60:40, a flow rate of 1.2 ml/min and column temperature maintained at 35°C. The effluents obtained were monitored at 255 nm with ultraviolet-visible detector. Results: The retention time of ellagic acid, quercetin, and piperine was found to be 1.65 min, 2.94 min, and 14.57 min, respectively. The linearity of ellagic acid, quercetin, and piperine was tested in the range of 6–14 ppm, 3–11 ppm, and 3–13 ppm, respectively. The correlation coefficient for ellagic acid, quercetin, and piperine was found to be 0.997, 0.993, and 0.99, respectively. The high recovery values (98–102%) indicate a satisfactory accuracy. The low percent relative standard deviation values in the precision study reveal that the method is precise. Conclusion: The developed method is novel, simple, precise, rapid, accurate, and reproducible for simultaneous quantitative estimation of ellagic acid, quercetin, and piperine in Ayurvedic formulations. Hence, the developed method can be used for quantitative analysis and quality control of extracts and commercial samples of other plant species and formulations containing these three markers.

scholarly journals High-Performance Thin-Layer Chromatography Densitometric Method for the Simultaneous Determination of Three Phenolic Acids in Syzygium aromaticum (L.) Merr. & Perry

2008 ◽  
Vol 91 (5) ◽  
pp. 1169-1173 ◽  
Author(s):  
Subha Rastogi ◽  
Madan M Pandey ◽  
Ajay K S Rawat
Keyword(s):  
Thin Layer ◽  
Gallic Acid ◽  
Simultaneous Determination ◽  
Caffeic Acid ◽  
Correlation Coefficient ◽  
Phenolic Acids ◽  
High Performance ◽  
Syringic Acid ◽  
Syzygium Aromaticum

Abstract A simple, precise, and rapid high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous determination of 3 phenolic acids, i.e., gallic acid, caffeic acid, and syringic acid, in the dried buds of Syzygium aromaticum, commonly known as clove. HPTLC was performed on silica gel 60F254 plates with tolueneethyl acetateformic acid (8 2 1) mobile phase and densitometric scanning at 280 nm. The method was validated for selectivity, linearity, precision, and repeatability. Instrumental precision coefficient of variation (CV) was 0.88, 0.93, and 0.98% and repeatability of the method (CV) was 0.76, 0.64, and 0.69% for gallic acid, caffeic acid, and syringic acid, respectively. The linear concentration ranges were 4003200 ng/spot with a correlation coefficient of 0.993 for gallic acid, 4403520 ng/spot with a correlation coefficient of 0.994 for caffeic acid, and 4004000 ng/spot with a correlation coefficient of 0.993 for syringic acid. The average recoveries of gallic acid, caffeic acid, and syringic acid were 96.3, 95.7, and 92.4%, respectively. Gallic acid, caffeic acid, and syringic acid were present at levels of 1.58, 0.06, and 0.05% (w/w), respectively, in S. aromaticum. This method is simple, accurate, precise, and economical and can be used for routine quality control.

scholarly journals DEVELOPMENT AND VALIDATION OF NOVEL RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF ELLAGIC ACID AND QUERCETIN IN AN AYURVEDIC FORMULATION

2018 ◽  
Vol 10 (4) ◽  
pp. 111 ◽  
Author(s):  
Vandana Jain ◽  
Sultana Shaikh
Keyword(s):  
Ellagic Acid ◽  
High Performance ◽  
Quantitative Estimation ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Column Temperature ◽  
Rp Hplc ◽  
Relative Standard ◽  
Liquid Chromatographic

Objective: To develop a novel, accurate, precise and linear reverse phase high performance liquid chromatographic (RP-HPLC) method for simultaneous qualitative and quantitative estimation of ellagic acid and quercetin in an ayurvedic formulation and validate as per international conference on harmonization (ICH) guidelines.Methods: In the present work, good chromatographic separation was achieved isocratically using a shim-pack HPLC C18 column (4.6 x 250 mm, 5μm) and a mobile phase consisting of 0.02 M potassium dihydrogen orthophosphate buffer (pH adjusted to 3.5 with orthophosphoric acid) and acetonitrile in the ratio 60:40, at flow rate of 1.2 ml/min and column temperature maintained at 35 °C. The effluents obtained were monitored at 255 nm with UV-visible detector.Results: The retention time of ellagic acid and quercetin were found to be 1.65 min and 2.94 min respectively. Linearity of ellagic acid and quercetin were tested in the range of 6-14 ppm and 3-11 ppm respectively. The correlation coefficient for ellagic acid and quercetin were 0.997 and 0.993 respectively. The high recovery values (98 %-102 %) indicate a satisfactory accuracy. The low percent relative standard deviation (% RSD) values in the precision study reveals that the method is precise.Conclusion: The developed method is novel, simple, precise, rapid, accurate and reproducible for simultaneous quantitative estimation of ellagic acid and quercetin in an ayurvedic formulation. Hence the developed method can be used for quantitative analysis and quality control of extracts and commercial samples of other plant species and formulation containing these two markers.

scholarly journals Determination of 5-nitro-2-furaldehyde as marker residue for nitrofurazone treatment in farmed shrimps and with addressing the use of a novel internal standard

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Qiang Wang ◽  
Xu-Feng Wang ◽  
Yong-Yuan Jiang ◽  
Zhi-Guang Li ◽  
Nan Cai ◽  
...  
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Ionization ◽  
Ultrasonic Manipulation

AbstractWe developed a significantly improved ultra-high performance liquid chromatography-tandem mass spectrometry method for determination of 5-nitro-2-furaldehyde (NF) as a surrogate using a novel internal standard for the detection of nitrofurazone. We used 2,4-dinitrophenylhydrazine derivatization and furfural as the internal standard. Derivatization was easily performed in HCl using ultrasonic manipulation for 5 min followed by liquid extraction using ethyl acetate. The samples were concentrated and purified using reverse phase and alumina cartridges in tandem. The derivatives were separated using a linear gradient elution on a C18 column with methanol and water as the mobile phase in negative ionization mode and multiple reaction monitoring. Under the optimized conditions, the calibration curves were linear from 0.2 to 20 μg/L with correlation coefficients >0.999. Mean recoveries were 80.8 to 104.4% with the intra- and inter-day relative standard deviations <15% at spiking levels of 0.1 to 10 μg/kg. The limits of detection and quantification were 0.05 and 0.1 μg/kg, respectively. This method is a robust tool for the identification and quantitative determination of NF in shrimp samples.

scholarly journals Screening of 49 antibiotic residues in aquatic products using modified QuEChERS sample preparation and UPLC-QToFMS analysis

2021 ◽  
Vol 3 ◽  
pp. e8
Author(s):  
Yao Gao ◽  
Tianwen Zhang ◽  
Shirong Huang ◽  
Xinxin Lin ◽  
Sisi Gong ◽  
...  
Keyword(s):  
Sample Preparation ◽  
Grass Carp ◽  
High Performance ◽  
Gradient Elution ◽  
Rapid Screening ◽  
Scylla Serrata ◽  
Penaeus Vannamei ◽  
Antibiotic Residues ◽  
Aquatic Products ◽  
Relative Standard

A precise analytical method was established for rapid screening of 49 antibiotic residues in aquatic products by ultra-high performance liquid chromatography-quadrupole time of flight mass spectrometry (UPLC-QToFMS). The quick, easy, cheap, effective, rugged and safe (QuEChERS) process was refined for effective sample preparation. The homogenized samples of aquatic products were extracted with 3% acetic acid in acetonitrile, salted out with anhydrous magnesium sulfate and sodium chloride, and cleaned up by octadecylsilane (C18) and primary-secondary amine (PSA) powder. Then, the purified samples were separated on a BEH C18 column using 0.1% formic acid and methanol as mobile phases by gradient elution, detected by MS under positive Electron Spray Ionization (ESI+) mode. The linear range of matrix-matched calibration curve was 1–100 μg/L for each compound with the correlation coefficients in the range of 0.9851–0.9999. The recoveries of target antibiotics at the different spiked levels ranged from 60.2% to 117.9% except for lincomycin hydrochloride, whereas relative standard deviations (RSDs) were between 1.6% and 14.0% except for sulfaguanidine in grass Carp, Penaeus vannamei and Scylla serrata matrices. The limits of detection (LODs) (S/N = 3) for the analytes were 0.05–2.40 μg/kg, 0.08–2.00 μg/kg and 0.10–2.27 μg/kg and the limits of quantification (LOQs) (S/N = 10) were 0.16–8.00 μg/kg, 0.25–6.66 μg/kg and 0.32–7.56 μg/kg in grass Carp, Penaeus vannamei and Scylla serrata, respectively. The method was successfully applied to grass Carp, Penaeus vannamei and Scylla serrata, demonstrating its ability for the determination of multi-categories antibiotic residues in aquatic products.

Qualitative and Quantitative Analysis of Flavonoids in Humulus scandens (Lour.)Merr. by UPLC-TQD and HPLC

2013 ◽  
Vol 295-298 ◽  
pp. 354-359 ◽  
Author(s):  
Xiao Wei Wang ◽  
Zhen Hua Liu ◽  
Rui Xiang Yu ◽  
De Hua Guo ◽  
Si Ming Zhu ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Hplc Method ◽  
Qualitative And Quantitative Analysis ◽  
Ultraviolet Detector ◽  
Relative Standard ◽  
Four Levels ◽  
Humulus Scandens

To qualify and quantify the flavonoids existing in Humulus scandens (Lour.)Merr., a Ultra performance liquid chromatography triple-quadrupole tandem mass spectrometer (UPLC-TQD) method was applied to preliminarily analyze the flavonoids exiting in Humulus. And a High performance liquid chromatography (HPLC) method was used to analyze the flavonoids existing in Humulus. Flavonoids in methanol extracts of Humulus were cleaned up by a C18 cartridge, separated by a PLASMA ODS column(5μm,250×4.6mm), with a gradient elution of methanol and 0.1% formic acid at a flow rate of 1 mL•min-1 . Analytes were detected with ultraviolet detector (UV) at 280nm. Flavonoids, including Epicatechin, Luteolin-7-O-Glucoside, Vitexin or Apigenin-7-glucoside, Morin hydrate or Quercetin dehydrate and Luteolin were found in Humulus according to the UPLC-TQD. Results of HPLC analysis showed the linear ranges of 11 flavonoids were 0.1mg•L-1-20mg•L-1 with the correlation coefficient (r) all above 0.9909. Limits of detection (signal/ noise=3) was 100Superscript text μg•L-1. The average recoveries of all the compounds spiked at four levels of 200μg•L-1, 500μg•L-1, 1 mg•L-1 and 1.5 mg•L-1 were in the ranges of 70.8%-112.1%, 74.6%-116.6%, 73.1%-110.6%, 73.7%-99.9%, with the corresponding relative standard deviation (RSD, n=6) of 2.5%-5.8%, 0.8%-4.3%, 0.8%-3.7%, 1.7%-3.8%, respectively. This method ,which was proved to be precise, sensitive and reliable, could be applied to analyze flavonoids in leaves.

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