scholarly journals Development and Validation of an Analytical Method for Carnosol, Carnosic Acid and Rosmarinic Acid in Food Matrices and Evaluation of the Antioxidant Activity of Rosemary Extract as a Food Additive

Antioxidants ◽  
2019 ◽  
Vol 8 (3) ◽  
pp. 76 ◽  
Author(s):  
Seung-Hyun Choi ◽  
Gill-Woong Jang ◽  
Sun-Il Choi ◽  
Tae-Dong Jung ◽  
Bong-Yeon Cho ◽  
...  
Keyword(s):  
Antioxidant Activity ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Acid Value ◽  
Food Additive ◽  
Carnosic Acid ◽  
Rosemary Extract ◽  
Relative Standard ◽  
Food Matrices

Antioxidants are used to prevent the oxidation of foods. When used for food additive purposes, the dosage should be regulated and the functionality evaluated to ensure stability. In this study, we performed a method validation for the quantitative analysis of rosemary extract residues and evaluated the antioxidant activity of rosemary extract in food matrices. The validated method was able to determine rosemary extract under the optimized high-performance liquid chromatography-photodiode array (HPLC-PDA) conditions. Furthermore, the antioxidant activity was evaluated by peroxide value, acid value, and in terms of the residual antioxidant levels in lard oil. For HPLC-PDA analysis, the limit of detection and quantification of rosemary extracts was ranged from 0.22 to 1.73 μg/mL, 0.66 to 5.23 μg/mL and the recoveries of the rosemary extracts ranged from 70.6 to 114.0%, with relative standard deviations of between 0.2% and 3.8%. In terms of antioxidant activity, carnosic acid performed better than carnosol. Furthermore, by evaluation of the residual antioxidant level using HPLC, we found that carnosic acid is more stable in lard oil than carnosol. These results indicate that rosemary extract can be used as an antioxidant and that the analytical method is suitable for the determination of rosemary extract in various food samples.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR ANALYSIS OF DEOXYARBUTININ ANHYDROUS EMULSION SYSTEM USING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 172-175 ◽  
Author(s):  
MUCHTARIDI MUCHTARIDI ◽  
IDA MUSFIROH ◽  
AHMAD FAUZI
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Emulsion System ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: The aim of this study is to develop a simple, precise and accurate analytical method of deoxyarbutin in anhydrous emulsion system preparation. Methods: The analysis was conducted using high-performance liquid chromatography (HPLC). Chromatographic analysis was carried out using a reversed phase-C18 column. The mobile consists of two phases methanol and water (60: 40 v/v) at a flow rate of 1.0 ml/min. The determinations were performed using UV detector set at 225 nm. All validation procedures were added with hydroquinone as an internal standard. Results: The method showed coefficient correlation is 0.9978, relative standard deviation (RSD) smaller than 2%, Limit of Detection (LOD) and Limit of Quantitation (LOQ) are 0.599 µg/ml and 1.817 µg/ml respectively. The total amount deoxyarbutin in anhydrous emulsion preparation is 1.964+0.02 % with 98% recovery percentage. Conclusion: The developed HPLC analytical method meets the validation criteria made by International Conference on Harmonisation (ICH).

scholarly journals Analytical method validation of reversed phase HPLC for quantitative analysis of tartrazine and auramine o in powder drinks

Food Research ◽  
2020 ◽  
Vol 4 (6) ◽  
pp. 2037-2041
Author(s):  
A.D. Lestari ◽  
A. Rohman ◽  
S. Martono
Keyword(s):  
Method Validation ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Coefficient Of Determination ◽  
Array Detector ◽  
Analytical Method Validation ◽  
Relative Standard ◽  
Auramine O

This study was aimed to perform analytical method validation of high-performance liquid chromatography (HPLC) technique using photo-diode array detector for the simultaneous determination of Tartrazine (TAR) and Auramine O (AUO) in powder drink products. TAR and AUO were analysed using Waters Shield C18 column (250 mm x 4.6 mm i.d., 5 µm) using PDA detector at 300-650 nm. The mobile phase used was acetonitrileammonium acetate 19 mM (86:14 v/v) delivered isocratically at a flow rate of 1.2 mL/ min. The optimized HPLC condition was subjected to analytical method validation by assessing some performance characteristics as guided by International Conference on Harmonization (ICH). The method was linear over the studied concentration ranges with the coefficient of determination (R2 ) of 0.999 and 0.997 for TAR and AUR with % intercept less than 2%, respectively. The developed method was sensitive with a limit of detection value of 0.0325 μg/mL and 0.1052 μg/mL for TAR and AUO, respectively. The method is also accurate and precise as indicated with acceptable recovery values of 99.0- 100.7% for TAR and 102.1-106.5% for AUO with relative standard deviation (RSD) values lower than those required by Association of Official Analytical Chemists’ (AOAC). The developed method is simple and can be used for routine analysis of TAR and AUO for quality assurance purposes of powder drinks.

scholarly journals Method Validation and Measurement Uncertainty Determination of Ethoxyquin and Antioxidant Activity in Paprika Seasonings and Paprika Sauces Frequently Consumed in South Korea

Separations ◽  
2020 ◽  
Vol 7 (4) ◽  
pp. 50
Author(s):  
Gill-Woong Jang ◽  
Sun-Il Choi ◽  
Xionggao Han ◽  
Xiao Men ◽  
Hee-Yeon Kwon ◽  
...  
Keyword(s):  
Antioxidant Activity ◽  
Liquid Chromatography ◽  
Quantitative Analysis ◽  
South Korea ◽  
Analytical Method ◽  
High Performance ◽  
Trade Association ◽  
Relative Standard ◽  
Photodiode Array

In this study, we investigated and validated a method for the quantitative analysis of ethoxyquin in paprika seasonings and sauces, which are frequently consumed in South Korea. Using this analytical method, we were able to confirm the presence of ethoxyquin under optimized high-performance liquid chromatography/photodiode array (HPLC-PDA) and liquid chromatography with tandem mass spectrometry conditions. Additionally, the antioxidant activity of ethoxyquin was assessed using the American Spice Trade Association values and its residual levels in paprika seasoning samples. The HPLC-PDA limits of detection and quantification for ethoxyquin were found to be 0.26 and 0.79 μg/mL, and 0.33 to 1.00 μg/mL, and the recoveries of ethoxyquin ranged from 86.75 to 101.70%, with relative standard deviations ranging from 0.31% to 3.59%. These results indicated that the analytical method in this study should be appropriate for the quantitative analysis of ethoxyquin in paprika seasoning and sauce matrices.

scholarly journals ANALYTICAL METHOD BY HPLC-DAD ALLOWS QUANTIFICATION OF QUERCETIN MARKER IN STANDARDIZED EXTRACT OF ANADENANTHERA COLUBRINA VAR. CEBIL

2017 ◽  
Vol 9 (8) ◽  
pp. 47
Author(s):  
Valmir Gomes De Souza ◽  
FabrÍcio Havy Dantas De Andrade ◽  
Fabio Santos De Souza ◽  
Rui Oliveira Macedo
Keyword(s):  
Analytical Method ◽  
High Performance ◽  
Room Temperature ◽  
Limit Of Detection ◽  
Array Detector ◽  
Diode Array Detector ◽  
Limit Of Quantification ◽  
Hydroalcoholic Extract ◽  
Relative Standard ◽  
Validation Parameters

Objective: The Anadenanthera colubrina (Vell.) Brennan var. cebil is a medicinal plant that has been used for the treatment of many diseases in the northeastern region of Brazil. This plant contains secondary metabolites such as quercetin, a flavonoid that is known by its antioxidant and anti-inflammatory effects. The aim of this work is to propose the validation of an analytical method using high-performance liquid chromatography with diode array detector (HPLC-DAD) for the quantification of quercetin and standardization of the hydroalcoholic extract (HAE) of A. colubrina.Methods: The A. colubrina extracts were prepared by the maceration process with powdered leaves at 20% weight: volume (w/v) and a hydroalcoholic solution at 50% volume: volume (v/v) for 120 h at room temperature. After pretreatment of the hydroalcoholic extract, the quercetin marker was used for quantification and proceeded to the evaluation of validation parameters for the method using HPLC-DAD.Results: The analytical method proved to be specific. Linear over the range 1.4–26.6 µg/ml, regression analysis showed a good correlation coefficient (R2= 0.999); the limit of detection (LOD) and the limit of quantification (LOQ) were 0.27 and 0.81 μg/ml respectively. The relative standard deviation (RSD) did not exceed 2.5% for precision. The proposed method was validated with an average recovery of 92.5–97.5%.Conclusion: The method was validated using HPLC-DAD, allowing the quantification of quercetin in the standardisation process of extracts and quality control of the herbal drug containing A. colubrina Phyto complex.

scholarly journals Development of a QuEChERS-Based UHPLC-MS/MS Method for Simultaneous Determination of Six Alternaria Toxins in Grapes

Toxins ◽  
2019 ◽  
Vol 11 (2) ◽  
pp. 87 ◽  
Author(s):  
Wenbo Guo ◽  
Kai Fan ◽  
Dongxia Nie ◽  
Jiajia Meng ◽  
Qingwen Huang ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Safe Procedure ◽  
Alternariol Monomethyl Ether ◽  
Limit Of Quantification ◽  
Alternaria Toxins ◽  
Relative Standard

A simple and reliable analytical method for the simultaneous determination of alternariol (AOH), altenuene (ALT), tentoxin (TEN), altenusin (ALS), tenuazonic acid (TeA), and alternariol monomethyl ether (AME) in grapes was developed by ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure with the extraction by acetonitrile and purification by sodium chloride (0.5 g) and anhydrous magnesium sulfate (0.5 g) was established to recover the six Alternaria toxins. After validation by determining the linearity (R2 > 0.99), recovery (77.8–101.6%), sensitivity (limit of detection in the range of 0.03–0.21 μg kg−1, and limit of quantification in the range of 0.09–0.48 μg kg−1), and precision (relative standard deviation (RSD) ≤ 12.9%), the analytical method was successfully applied to reveal the contamination state of Alternaria toxins in grapes. Among 56 grape samples, 40 (incidence of 71.4%) were contaminated with Alternaria toxins. TEN was the most frequently found mycotoxin (37.5%), with a concentration range of 0.10–1.64 μg kg−1, followed by TeA (28.6%) and AOH (26.8%). ALT (10.7%), AME (3.6%), and ALS (5.4%) were also detected in some samples. To the best of our knowledge, this is the first report about the Alternaria toxins contamination in grapes in China.

scholarly journals Physicochemical Equivalence and Validation of an HPLC Analytical Method for the Quantification of Glibenclamide and Its Sulfonamide Impurity in Prescribed Glibenclamide Tablets in Nigeria

2019 ◽  
pp. 1-17
Author(s):  
Josephine Oluwagbemisola Tella ◽  
Saheed Oluwasina Oseni ◽  
Basheeru Kazeem Adebayo
Keyword(s):  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Crushing Strength ◽  
Acceptable Limit ◽  
Drug Products ◽  
Relative Standard ◽  
Physicochemical Evaluation

Objective: To investigate the physicochemical equivalence of four brands of commercially available glibenclamide tablets in Nigeria and to develop a validation method using HPLC for the quantitative determination of glibenclamide and its sulfonamide impurity present in these tablets. Methods: Uniformity of weight, friability tests, hardness/crushing strength, dissolution, and disintegration tests were carried out on tablets/drug samples of each brand. Their functional groups were determined and compared with pure glibenclamide sample (reference standard) using Fourier Transform Infrared Spectroscopy (FTIR) between a range of 4000cm-1 to 400cm-1. High-Performance Liquid Chromatography (HPLC) was used to determine the percentage of glibenclamide and its sulfonamide impurity present in each tablet brand. Results: From the physicochemical evaluation of the four brands of glibenclamide tablets tested, the brands passed all the British Pharmacopeia specifications, but they all failed the hardness/crushing strength tests and one of the brands failed the assay test requirement for drug content. The developed HPLC method had a percentage recovery between the acceptable limit of 95-105% with percentage relative standard deviation (%RSD) of < 3% while the precision of the method was 0.102% and 0.383% for glibenclamide and its sulfonamide impurity, respectively. The Limit of Detection (LOD) and Limit of Quantification (LOQ) of the developed analytical method for the four brands were 0.075µg/ml and 0.227µg/ml for glibenclamide while that of sulfonamide impurity were 0.114µg/ml and 0.345µg/ml, respectively. In addition, the percentage impurity of sulfonamide in all the brands was less than the acceptable limit of 1%. Conclusion: The results from the physicochemical evaluation of the glibenclamide brands justified the need for constant monitoring of marketed drug products. The results obtained from the HPLC quantification method developed for this study show that our data is reproducible based on the linearity, precision, and accuracy of data generated for glibenclamide and its sulfonamide impurity in the four brands of glibenclamide tablets prescribed to DM patients in Nigeria, which were judged to be satisfactory at the time of this study.

Calcium/Copper alginate framework doped with CuO nano-particles as a novel adsorbent for micro-extraction of benzodiazepines from human serum

2020 ◽  
Vol 16 ◽  
Author(s):  
Nadereh Rahbar ◽  
Fatemeh Ahmadi ◽  
Zahra Ramezani ◽  
Masoumeh Nourani
Keyword(s):  
Human Serum ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Nano Particles ◽  
Limit Of Quantification ◽  
Analytical Methodology ◽  
Fiber Fabrication ◽  
Relative Standard ◽  
Green Procedure

Background: Sample preparation is one of the most challenging phases in pharmaceutical analysis, especially in biological matrices, affecting the whole analytical methodology. Objective: In this study, a new Ca(II)/Cu(II)/alginate/CuO nanoparticles hydrogel fiber (CCACHF) was synthesized through a simple, green procedure and applied for fiber micro solid phase extraction (FMSPE) of diazepam (DIZ) and oxazepam (OXZ) as model drugs prior to high-performance liquid chromatography-UV detection (HPLC-UV). Methods: Composition and morphology of the prepared fiber were characterized and the effect of main parameters on the fiber fabrication and extraction efficiency have been studied and optimized. Results: In optimal conditions, calibration curves were linear ranging between 0.1–500 µg L−1 with regression coefficients of 0.9938 and 0.9968. Limit of detection (LOD) (S/N=3) and limit of quantification (LOQ) (S/N=10) of the technique for DIZ and OXZ were 0.03 to 0.1 µg L−1. Within-day and between-day relative standard deviations (RSDs) for DIZ and OXZ were 6.0–12.5% and 3.3–9.4%, respectively. Conclusion: The fabricated adsorbent has been substantially employed to extraction of selected benzo-diazepines (BZDs) from human serum real specimens and the obtained recoveries were also satisfactory (82.1-109.7%).

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

scholarly journals Validation of high performance liquid chromatography method for determination of meloxicam loaded PEGylated nanocapsules

2015 ◽  
Vol 51 (4) ◽  
pp. 823-832 ◽  
Author(s):  
Francine Rodrigues Ianiski ◽  
Luciane Varini Laporta ◽  
Alexandre Machado Rubim ◽  
Cristiane Luchese
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Zeta Potential ◽  
Analytical Method ◽  
High Performance ◽  
Ph Value ◽  
Hplc Method ◽  
Polydispersity Index ◽  
Size Distributions ◽  
Relative Standard

abstract A method to ensure that an analytical method will produce reliable and interpretable information about the sample must first be validated, making sure that the results can be trusted and traced. In this study, we propose to validate an analytical high performance liquid chromatography (HPLC) method for the quantitation of meloxicam loaded PEGylated nanocapsules(M-PEGNC). We performed a validation study, evaluated parameters including specificity, linearity, quantification limit, detection limit, accuracy, precision and robustness. PEGylated nanocapsules were prepared by interfacial deposition of preformed polymer, and the particle size, polydispersity index, zeta potential, pH value and encapsulation efficiency were characterized. The proposed HPLC method provides selective, linear results in the range of 1.0-40.0 μg/mL; quantification and detection limits were 1.78 μg/mL and 0.59 μg/mL, respectively; relative standard deviation for repeatability was 1.35% and intermediate precision was 0.41% and 0.61% for analyst 1 and analyst 2, respectively; accuracy between 99.23 and 101.79%; robustness between 97.13 and 98.45% for the quantification of M-PEGNC. Mean particle diameters were 261 ± 13 nm and 249 ± 20 nm, polydispersity index was 0.15 ± 0.07 and 0.17 ± 0.06, pH values were 5.0 ± 0.2 and 5.2 ± 0.1, and zeta-potential values were -37.9 ± 3.2 mV e -31.8 ± 2.8 mV for M-PEGNC and placebo(B-PEGNC), respectively. In conclusion, the proposed analytical method is suitable for the quality control of M-PEGNC. Moreover, suspensions showed monomodal size distributions and low polydispersity index indicating high homogeneity of formulations with narrow size distributions, and appropriate pH and zeta potential. The extraction process was efficient for release of meloxicam from nanostructured systems.

Determination of Potential Genotoxic Impurity, 5-Amino-2-Chloropyridine, in Active Pharmaceutical Ingredient Using the HPLC-UV System

2020 ◽  
Author(s):  
Murat Soyseven ◽  
Rüstem Keçili ◽  
Hassan Y Aboul-Enein ◽  
Göksel Arli
Keyword(s):  
Analytical Method ◽  
High Performance ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Detection System ◽  
Active Pharmaceutical Ingredient ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Water Ph

Abstract A novel analytical method, based on high-performance liquid chromatography with a UV (HPLC-UV) detection system for the sensitive detection of a genotoxic impurity (GTI) 5-amino-2-chloropyridine (5A2Cl) in a model active pharmaceutical ingredient (API) tenoxicam (TNX), has been developed and validated. The HPLC-UV method was used for the determination of GTI 5A2Cl in API TNX. The compounds were separated using a mobile phase composed of water (pH 3 adjusted with orthophosphoric acid): MeOH, (50:50: v/v) on a C18 column (150 × 4.6 mm i.d., 2.7 μm) at a flow rate of 0.7 mL min−1. Detection was carried out in the 254 nm wavelength. Column temperature was maintained at 40°C during the analyses and 10 μL volume was injected into the HPLC-UV system. The method was validated in the range of 1–40 μg mL−1. The obtained calibration curves for the GTI compound was found linear with equation, y = 40766x − 1125,6 (R2 = 0.999). The developed analytical method toward the target compounds was accurate, and the achieved limit of detection and limit of quantification values for the target compound 5A2Cl were 0.015 and 0.048 μg mL−1, respectively. The recovery values were calculated and found to be between 98.80 and 100.03%. The developed RP-HPLC-UV analytical method in this research is accurate, precise, rapid, simple and appropriate for the sensitive analysis of target GTI 5A2Cl in model API TNX.

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