High-Performance Liquid Chromatography Determination of Acrylamide after Its Extraction from Potato Chips

2019 ◽  
Vol 25 (4) ◽  
pp. 338-344
Author(s):  
Maryam Ghalebi ◽  
Samin Hamidi ◽  
Mahboob Nemati
Keyword(s):  
Organic Solvent ◽  
Organic Phase ◽  
High Performance ◽  
Single Step ◽  
Potato Chips ◽  
Process Efficiency ◽  
Local Market ◽  
Good Precision ◽  
Time Saving ◽  
Relative Standard

Background: Acrylamide is a known carcinogenic product that has been found among the substances such as potato chips which to be processed under the heat-treatment. In order to extract amounts of acrylamide from fried chips in market, an ultrasound-assisted liquid– liquid extraction (UA-LLE) technique is proposed. The UA-LLE coupled LLE and ultrasonication in a single step. Methods: Chips samples were dissolved in an extracting organic solvent using ultrasonication to prompt transferring of acrylamide into the organic phase. As a result, the extraction time and process efficiency were significantly enhanced through increasing the collision power and mass transfer between grounded chips and organic phase. Results: Important parameters affecting the extraction efficiency such as kind of organic solvent and its volume, re-dissolving solvent and pH were optimized. This newly proposed method has been applied to determine the trace acrylamide in potato chips samples purchased from local market. Conclusion: UA-LLE is a handy, economic and time-saving method, with high extraction yield (over 103% average recovery) and good precision (lower than 15% relative standard deviation, RSD). Most importantly, it seems this method to be an ideal pre-treatment method for the extraction of acrylamide in food matrix in food quality control laboratories.

scholarly journals SLE Single-Step Purification and HPLC Isolation Method for Sterols and Triterpenic Dialcohols Analysis from Olive Oil

Foods ◽  
2021 ◽  
Vol 10 (9) ◽  
pp. 2019
Author(s):  
Manuel León-Camacho ◽  
María del Carmen Pérez-Camino
Keyword(s):  
High Performance ◽  
Small Sample Size ◽  
Reference Value ◽  
Fats And Oils ◽  
Single Step ◽  
Small Sample ◽  
Analytical Control ◽  
Unsaponifiable Fraction ◽  
Time Saving ◽  
Relative Standard

The unsaponifiable fraction of oils and fats constitutes a very small fraction but it is an essential part of the healthy properties of some specific oils. It is a complex fraction formed by a large number of minor compounds and it is a source of information to characterize and authenticate the oil sample. Specially, the composition of sterols of any oil or fat is a distinctive feature of itself and, therefore, it has become a useful tool for detecting contaminants and adulterants in oils. A new supported liquid extraction (SLE) technique for the analysis and characterization of the unsaponifiable fraction of fats and oils is proposed. The SLE system includes, as a stationary phase, a combination of adsorbent materials which allow a highly purified unsaponifiable matter ready to be isolated by high performance liquid chromatography (HPLC) and quantified by gas chromatography (GC). This method ensures the removal of fatty acids, avoiding possible interferences and making the analysis of sterols and triterpenic dialcohols easier. The procedure uses a small sample size (0.2 g), reduces the volume of solvents and reagents, and reduces the handling of samples subjected to analytical control. All this is achieved without losing either precision—a relative standard deviation of each compound lower than the reference value (≤16.4%)—or recovery, being for all compounds higher than 88.00%. Therefore, this new technique represents a significant economic and time saving in business control laboratories, a larger productivity and enhancement of working safety.

Fluoroimmunoassay Based on FITC-Labeled Antibody for the Determination of Estradiol

2014 ◽  
Vol 960-961 ◽  
pp. 3-6
Author(s):  
Long Jun Wang ◽  
Wei Li Xue ◽  
Ling Yun Du
Keyword(s):  
Human Urine ◽  
High Performance ◽  
Solid Phase ◽  
High Sensitivity ◽  
Good Precision ◽  
Experimental Conditions ◽  
Time Saving ◽  
Relevant Variable ◽  
Relative Standard

A new fluorescence immunoassay with high sensitivity, time-saving, good precision and reliablility was proposed for the determination of estradiol (E2) in human urine. The complex of FITC-labeled anti-E2antibody was produced and regarded as a probe in this system. Ninety-six microplate was coated with ovalbumin conjugated E2antigen as solid phase for the immunoassay. The method parameters affecting the determination, such as the concentration of immunoreagents, pH, and other relevant variable conditions upon the immunoassay were studied and optimized systematically. Under the optimal experimental conditions, it was found that the proposed method exhibited high performance with the detection limit of 9.2 pg/mL, and the linear range of determination of 0.01-1000 ng/mL. The recoveries were 93.58-105.82% with the relative standard deviations (RSD) 5.52-7.09%. The proposed method has been used for the determination of E2in human urine with satisfactory results, and may be expected to find wide application in other environmental samples.

scholarly journals High-Performance Thin-Layer Chromatography with Densitometry for the Determination of Ciprofloxacin and Impurities in Drugs

2005 ◽  
Vol 88 (5) ◽  
pp. 1530-1536 ◽  
Author(s):  
Jan Krzek ◽  
Urszula Hubicka ◽  
Justyna Szczepańczyk
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
High Sensitivity ◽  
Good Precision ◽  
Relative Standard ◽  
Tlc Plates ◽  
Quantitative Analyses

Abstract A thin-layer chromatographic (TLC)-densitometric method has been developed for identification and quantification of ciprofloxacin (Rf = 0.61) and an ethylenediamine compound (Rf = 0.42), a desfluoro compound (Rf = 0.48), by-compound A (Rf = 0.53), and fluoroquinolonic acid (Rf = 0.68) as ciprofloxacin degradation products in pharmaceutical preparations. By using chloroform–methanol–25% ammonia (43 + 43 + 14, v/v/v) as the mobile phase and silica gel 60 F254 high-performance TLC plates as the stationary phase, it was possible to separate individual constituents that, when subjected to ultraviolet (UV) densitometric analysis at 330 nm for fluoroquinolonic acid and 277 nm for the other compounds, gave well developed peaks allowing easy qualitative and quantitative analyses. DMSO–methanol (1 + 1) was used to extract drug constituents. The method showed high sensitivity (limit of detection 10 to 44 ng), a wide linearity range (3 to 20 μg/mL), and good precision (2.32 to 6.46% relative standard deviation) and accuracy (percentage recoveries 98.62 to 101.52%) for individual constituents.

scholarly journals An integrated targeted and untargeted approach for the analysis of ergot alkaloids in cereals using UHPLC – hybrid quadrupole time-of-flight mass spectrometry

2015 ◽  
Vol 8 (5) ◽  
pp. 653-666 ◽  
Author(s):  
N. Arroyo-Manzanares ◽  
J. Diana Di Mavungu ◽  
V. Uka ◽  
L. Gámiz-Gracia ◽  
A.M. García-Campaña ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance ◽  
Time Of Flight ◽  
Ergot Alkaloids ◽  
Good Precision ◽  
Method Performance ◽  
Analytical Strategy ◽  
Flight Mass Spectrometry ◽  
Detection And Identification ◽  
Relative Standard

An ultra-high performance liquid chromatography hybrid quadrupole – time of flight (Q-TOF) mass spectrometry (MS) method is described for the simultaneous quantitative determination of common ergot alkaloids and the screening, detection and identification of unexpected (less studied or novel) members of this class of toxic fungal secondary metabolites. The employed analytical strategy involves an untargeted data acquisition (consisting of full scan TOF MS survey and information dependent acquisition MS/MS scans) and the processing of data using both targeted and untargeted approaches. Method performance characteristics for the quantitative analysis of 6 common ergot alkaloids i.e. ergometrine, ergosine, ergotamine, ergocornine, ergocristine, ergokryptine and their corresponding epimers in rye were comparable to those previously reported for triple-quadrupole (QqQ) MS/MS. The method limits of quantification (LOQ) were in the range from 3 to 19 μg/kg, and good linearity was observed for the different ergot alkaloids in the range from LOQ to 1000 μg/kg. Furthermore, the method demonstrated good precision (relative standard deviations at 50 μg/kg not higher than 14.6 and 16.2% for the intra-day and inter-day precision, respectively), and the trueness values at different concentration levels were all between 89 and 115%. The method was applied for the analysis of a set of 17 rye samples and demonstrated the presence of these ergot alkaloids in the range from <LOQ to 2,811 μg/kg. Further mining of the same data based on a ‘non-targeted peak finding’ algorithm and the use of full MS and MS/MS accurate mass data allowed the detection and identification of 19 ergot alkaloids that are commonly not included in most analytical methods using QqQ instruments. Some of these alkaloids are reported for the first time in naturally contaminated samples.

scholarly journals A Strategy for Quality Control of Vespa magnifica (Smith) Venom Based on HPLC Fingerprint Analysis and Multi-Component Separation Combined with Quantitative Analysis

Molecules ◽  
2019 ◽  
Vol 24 (16) ◽  
pp. 2920 ◽  
Author(s):  
Si-Tong Zhou ◽  
Kai Luan ◽  
Lian-Li Ni ◽  
Ying Wang ◽  
Shi-Meng Yuan ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
High Performance ◽  
Principal Component ◽  
Good Precision ◽  
Fingerprint Analysis ◽  
Wasp Venom ◽  
Chemical Fingerprint ◽  
Hplc Fingerprint ◽  
Relative Standard

As a folk medicine of the Jingpo minority in Yunnan province, the venom of Vespa magnifica has been commonly used for the treatment of rheumatoid arthritis. Quality standardization of the wasp venom is a necessary step for its pharmaceutical research and development. To control the quality of the wasp venom, a method based on high-performance liquid chromatography (HPLC) was developed for chemical fingerprint analysis. In the chromatographic fingerprinting, chemometrics procedures, including similarity analysis (SA), hierarchical clustering analysis (HCA), and principal component analysis (PCA), were applied to classify 134 batches (S1–S134) of wasp venom from different origins. The HPLC fingerprint method displayed good precision (Relative standard deviation, RSD < 0.27%), stability (in 16 h, RSD < 0.34%), and repeatability (RSD < 1.00%). Simultaneously, four compounds (VMS1, VMS2, VMS3, and VMS4) in the wasp venom were purified and identified. VMS1 was 5-hydroxytryptamine, and the other compounds were three peptides that were sequenced as follows: Gly–Arg–Pro–Hyp–Gly–Phe–Ser–Pro–Phe–Arg–Ile–Asp–NH2 (VMS2), Ile–Asn–Leu–Lys–Ala–Ile–Ala–Ala–Leu–Ala–Lys–Lys–Leu–Leu–NH2 (VMS3), and Phe–Leu–Pro–Ile–Ile–Gly–Lys–Leu–Leu–Ser–Gly–Leu–Leu–NH2 (VMS4). The quantifications for these components were 110.2 mg/g, 26.9 mg/g, 216.3 mg/g, and 58.0 mg/g, respectively. The results of this work indicated that the combination of the chemical fingerprint and quantitative analysis offers a reasonable way to evaluate the quality of wasp venom.

scholarly journals Analysis of Flavonol Aglycones and Terpenelactones in Ginkgo biloba Extract: A Comparison of High-Performance Thin-Layer Chromatography and Column High-Performance Liquid Chromatography

2007 ◽  
Vol 90 (5) ◽  
pp. 1203-1209 ◽  
Author(s):  
Dean E Gray ◽  
Dale Messer ◽  
Andrew Porter ◽  
Brian Hefner ◽  
Dama Logan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Ginkgo Biloba ◽  
High Performance ◽  
Flavonol Glycosides ◽  
Time Saving ◽  
Relative Standard ◽  
Layer Chromatography

Abstract Advancements in automated high-performance thin-layer chromatography (HPTLC) have made it feasible to assess its use for the quantitative analysis of marker compounds in botanical preparations. We report here the findings of method comparisons for the terpenelactones and flavonol aglycones by column high-performance liquid chromatography (HPLC) with evaporative light scattering and UV detection, and HPTLC with a scanning densitometer. For the HPTLC assay of terpenelactones, total bilobalide, ginkgolide A, and ginkgolide B consistently achieved &lt;70 of the total determined using HPLC, regardless of variations to postchromatographic derivatization time and temperature. Accuracy testing showed the possibility of a matrix interference. In contrast, a good relationship (95) was determined between HPTLC and HPLC for determination of total flavonol glycosides (calculated from combined quercetin, kaempferol, and isorhamnetin) from an acid-hydrolyzed Ginkgo biloba L. (GBE) sample. The HPTLC flavonol aglycone method also performed well in terms of accuracy (overall average of 96 recovery for the 3 aglycones) and consecutive plate repeatability (overall percent relative standard deviation of 4.4). It is demonstrated that HPTLC can be a time-saving complement to HPLC for routine analysis of the flavonol glycosides in GBE.

scholarly journals Simultaneous quantifications of four purine derivatives biomarkers in cow milk by SPE HPLC-DAD

2021 ◽  
Vol 39 (No. 2) ◽  
pp. 122-130
Author(s):  
Mihaela Vlassa ◽  
Miuta FILIP ◽  
Catalin DRAGOMIR
Keyword(s):  
Uric Acid ◽  
High Performance ◽  
Solid Phase ◽  
Cow Milk ◽  
Good Precision ◽  
Purine Derivatives ◽  
Buffer Solution ◽  
Solution Ph ◽  
Relative Standard ◽  
Array Detection

In this study, simultaneous quantification of allantoin, uric acid, xanthine, and hypoxanthine in cow milk by solid phase extraction (SPE) and high performance liquid chromatography-diode array detection (HPLC-DAD) method was perform. Five different SPE cartridges were tested in order to evaluate the isolation of purine derivatives (PD) from cow milk. Chromatography was carried out on ODS-2 Hypersil column and 0.05 M (NH<sub>4</sub>)<sub>2</sub>HPO<sub>4</sub> buffer solution (pH = 7.76) as mobile phase. The HPLC-DAD validated method showed a linearity with regression coefficients higher than 0.999 and the limits of detection and quantification with values in the range 0.09–0.74 µg mL<sup>–1</sup> and 0.27–2.24 µg mL<sup>–1</sup>, respectively. The method showed good precision with a relative standard deviation (RSD) below 4.48%, while the accuracy ranged from 95.34 to 104.47% for all analytes. The best recovery degree of PD by SPE were obtained on Strata SCX cartridge for xanthine (87.79%) and hypoxanthine (89.02%); on Strata NH<sub>2</sub> for allantoin (35.09%) and on Strata C8 for uric acid (101.08%). Finally, the HPLC-DAD method with SPE on SCX cartridges was applied to quantify the PD in a batch of thirty cow milk samples.

scholarly journals A Validated Ultrasound-Assisted Extraction Coupled with SPE-HPLC-DAD for the Determination of Flavonoids in By-Products of Plant Origin: An Application Study for the Valorization of the Walnut Septum Membrane

Molecules ◽  
2021 ◽  
Vol 26 (21) ◽  
pp. 6418
Author(s):  
Natasa P. Kalogiouri ◽  
Victoria F. Samanidou
Keyword(s):  
Functional Properties ◽  
High Performance ◽  
Solid Phase ◽  
Good Precision ◽  
Bioactive Constituents ◽  
Ultrasound Assisted Extraction ◽  
Relative Standard ◽  
Ultrasound Assisted ◽  
Flavonoid Fraction

Walnut byproducts have been shown to exert functional properties, but the literature on their bioactive content is still scarce. Among walnut byproducts, walnut septum is a dry ligneous diaphragm tissue that divides the two halves of the kernel, exhibiting nutritional and medicinal properties. These functional properties are owing to its flavonoid content, and in order to explore the flavonoid fraction, an ultrasound-assisted (UAE) protocol was combined with solid phase extraction (SPE) and coupled to high-performance liquid chromatography with diode array detection (HPLC-DAD) for the determination of flavonoids in Greek walnut septa membranes belonging to Chandler, Vina, and Franquette varieties. The proposed UAE-SPE-HPLC-DAD method was validated and the relative standard deviations (RSD%) of the within-day and between-day assays were lower than 6.2 and 8.5, respectively, showing good precision, and high accuracy ranging from 90.8 (apigenin) to 97.5% (catechin) for within-day assay, and from 88.5 (myricetin) to 96.2% (catechin) for between-day assay. Overall, seven flavonoids were determined (catechin, rutin, myricetin, luteolin, quercetin, apigenin, and kaempferol) suggesting that the walnut septum is a rich source of bioactive constituents. The quantification results were further processed using ANOVA analysis to examine if there are statistically significant differences between the concentration of each flavonoid and the variety of the walnut septum.

scholarly journals VALIDATION OF ASSAY PROCEDURES OF AFOBAZOLEIN MICROCAPSULES

2017 ◽  
Vol 9 (5) ◽  
pp. 278
Author(s):  
Polkovnikova Yulia Aleksandrovna ◽  
Slivkin Aleksei Ivanovich ◽  
Halahakoon Amila Jeewantha
Keyword(s):  
High Performance ◽  
Analytical Procedure ◽  
Ammonium Phosphate ◽  
Hplc Method ◽  
Good Precision ◽  
Assay Procedure ◽  
Analytical Curve ◽  
Validation Criteria ◽  
Relative Standard ◽  
Sufficient Precision

Objective: The aim of this work was focused on a simple, rapid, accurate and sensitive method for quantitative analysis of afobazole in microcapsules (afb-m) using high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection.Methods: The analytical procedure was based on the fractionation characteristics of the afobazole in the chromatography column. The chromatography parameters «Zorbax extend-C18» column (150×2.1 mm i.d. 5 µm particle size), at 40 °C. The isocratic mobile phase was 5.0 M ammonium phosphate buffer (pH 7.0): acetonitrile (30:70; v/v) at a flow rate of at 1.0 ml. min-1. The determinations were performed using UV-Vis detector set at 220 nm.Results: An assay procedure for afb-m has been validated from indices, such as specificity, correctness, precision, and linearity. The registered retention time of the afobazole stock solution and the sample solution was 1.5 min. The determined accuracy of the method was in the range of 99.67%-100.67%. The analytical curve was linear (r2-0.9996) over a wide concentration range (50%-150%). The method showed sufficient precision, with a relative standard deviation (RSD) smaller than 2%.Conclusion: The HPLC method developed in this study showed specificity and selectivity with linearity in the working range and good precision and accuracy, making it very suitable for quantification of afb-m. The developed assay procedure of afb-m was meeting all the requirements of ICH validation criteria and can be applied for standardisation drug form afb-m.

Determination of Organic Impurities in Anthraquinone Color Additives D&C Violet No. 2 and D&C Green No. 6 by Ultra-High Performance Liquid Chromatography

2017 ◽  
Vol 100 (1) ◽  
pp. 230-235 ◽  
Author(s):  
H H Wendy Yang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Correlation Coefficients ◽  
Photodiode Array Detection ◽  
Time Saving ◽  
Organic Impurities ◽  
Relative Standard ◽  
Photodiode Array ◽  
Color Additive

Abstract A new practical and time-saving ultra-high performance liquid chromatography (UHPLC) method has been developed for determining the organic impurities in the anthraquinone color additives D&C Violet No. 2 and D&C Green No. 6. The impurities determined are p-toluidine, 1-hydroxyanthraquinone, 1,4-dihydroxyanthraquinone, and two subsidiary colors. The newly developed UHPLC method uses a 1.7-μ particle size C-18 column, 0.1 M ammonium acetate and acetonitrile aseluents, and photodiode array detection. For the quantification of the impurities, six-point calibration curves were used with correlation coefficients that ranged from 0.9974 to 0.9998. Recoveries of impurities ranged from 99 to 104%. Relative standard deviations ranged from 0.81 to 4.29%. The limits of detection for the impurities ranged from 0.0067% to0.216%. Samples from sixteen batches of each color additive were analyzed, and the results favorably compared with the results obtained by gravity-elution column chromatography, thin-layer chromatography, and isooctane extraction. Unlike with those other methods, use of the UHPLC method permits all of the impurities to be determined in a single analysis, while also reducing the amount of organic waste and saving timeand labor. The method is expected to be implemented by the U.S. Food and Drug Administration for analysis of color additive samples submitted for batch certification.

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