scholarly journals Validation of an analytical method for the determination of acrylamide in potato chips and french fries

2021 ◽  
Vol 45 (1) ◽  
pp. 69-85
Author(s):  
Mioara Negoiță ◽  
Adriana Laura Mihai ◽  
Gabriela-Andreea Horneț
Keyword(s):  
Ethyl Acetate ◽  
Solid Phase ◽  
Potato Chips ◽  
French Fries ◽  
Performance Criteria ◽  
Good Precision ◽  
Proficiency Tests ◽  
Hexane Extraction ◽  
Commission Regulation

The aim of this study was to validate a GC-MS/MS method for determining acrylamide (AA) in potato-based products by using the solid-phase extraction (SPE) clean-up. The method consisted in defatting the sample (potato chips, French fries) with hexane, extraction of AA in water, centrifugation, followed by AA purification on two SPE columns. The purified extract was derivatized with bromine compounds, then extracted with ethyl acetate: hexane mixture. The residue dissolved in ethyl acetate and triethylamine was injected into the GC-MS/MS. The method showed a good precision (RSDr= 1.13- 4.26%; RSDR= 1.19- 8.84%) and accuracy (recovery= 85.64- 109.22%). The precision of the results was demonstrated by participation in two proficiency tests launched by the FAPAS® program, yielding z-scores of -0.8 (for pre-cooked French fries) and 0 (for potato crisps). Good sensitivity was achieved for potato chips with a LOD and LOQ of 6.94 and 20.83 μg/kg, while for French fries, it was 10.29 and 30.87 μg/kg, respectively. When applying the method on potato chips sample, the AA level varied between undetectable and 1504.93 μg/kg, while for French fries was between 31.45- 371.30 μg/kg. The method fulfilled the performance criteria of Commission Regulation EU 2017/2158 for the determination of AA in potato-based products.

Determination of Organophosphorus Nematicide Residues in Banana-Field Soils by Gas Chromatography/Mass Spectrometry

1994 ◽  
Vol 77 (6) ◽  
pp. 1580-1586
Author(s):  
Jean-François Cooper ◽  
Shan-Qiang Zheng ◽  
Nigel R Wynn ◽  
Louis Palcy
Keyword(s):  
Ethyl Acetate ◽  
West Indies ◽  
Solid Phase ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Solvent Mixtures ◽  
Phase Extraction ◽  
Field Soils ◽  
Chromatographic Mass

Abstract Gas chromatographic/mass spectrometric (GC/MS) methodology is presented for the determination, in banana-field soils, of the 4 most used organophosphorus nematicides in Martinique (French West Indies): cadusafos (Rugby), ethoprophos (Mocap), isazophos (Miral), and fenamiphos (Nemacur). After extraction with 2 successive solvent mixtures, ethyl acetate–dichloromethane (8 + 2, v/v) and ethyl acetate–acetone (7 + 3, v/v), cleanup was performed using solid-phase extraction cartridges (silica SPE). Fenamiphos and its metabolites were separated in the second eluate and then oxidized to sulfone. Analysis was performed by GC/MS in fragmentometric mode. Recoveries varied from about 75 to 90%. Limits of quantitation varied from 4 to 20 μg/kg fresh soil sample, depending on the nematicide.

A Rapid Multiresidue Screen for Organophosphorus, Organochlorine, and N-Methyl Carbamate Insecticides in Plant and Animal Tissues

1994 ◽  
Vol 77 (5) ◽  
pp. 1263-1274 ◽  
Author(s):  
Dirk M Holstege ◽  
David L Scharberg ◽  
Elizabeth R Tor ◽  
Laura C Hart ◽  
Francis D Galey
Keyword(s):  
Ethyl Acetate ◽  
Solid Phase ◽  
Gel Permeation Chromatography ◽  
Bovine Liver ◽  
Animal Tissues ◽  
Average Recovery ◽  
Carbamate Insecticides ◽  
High Lipid ◽  
Level Method

Abstract A multiresidue screen for the quantitative determination of 43 organ op hosphorus, 17 orga no-chlorine, and 11 N-methyl carbamate insecticides in 10 g of plant or animal tissues is described. The insecticides are extracted with 5% ethanol in ethyl acetate (v/v). Samples with high lipid content are cleaned up by automated gel permeation chromatography with a 30% ethyl acetate in hexane (v/v) eluant and in-line silica gel minicolumns. Highly pigmented samples are cleaned up with class-specific solid-phase extraction columns. The concentrated extracts are analyzed by selective detection with gas chromatography or liquid chromatography. Recovery of 71 insecticides ranged from 77 to 113%. Analysis of fortified bovine liver (n = 5) resulted in an average recovery of 96 ± 4% at the 0.5 to 0.05 μg/g level. Analysis of fortified alfalfa hay (n = 5) resulted in a mean recovery of 94 ± 4% at the 0.06 to 0.5 μg/g level, and analysis of fortified fresh tomatoes (n = 5) resulted in an average recovery of 97 ± 3% at the 0.06 to 0.5 μg/g level. Method detection limits ranged from 0.02 to 0.5 μg/g for the compounds studied with a nominal 10 g sample.

A new reagent strip (Visidex) for determination of glucose in whole blood.

1983 ◽  
Vol 29 (3) ◽  
pp. 438-446 ◽  
Author(s):  
M J Sherwood ◽  
M E Warchal ◽  
S T Chen
Keyword(s):  
Whole Blood ◽  
Solid Phase ◽  
Sample Volume ◽  
Operator Technique ◽  
Good Precision ◽  
Visual Resolution ◽  
Color Development ◽  
Color Scale ◽  
High Concentrations

Abstract A new solid-phase reagent strip for determination of glucose in whole blood, Visidex, has been developed specifically for visual use in conjunction with a calibrated color scale. Two reagent pads are used, each formulated for a different portion of the range of clinical values, to maximize the visual resolution available to the user. Colorimetric examination of reacted reagent pads indicated that the label color blocks match closely the appearance of the reagent pads; that the reagent pads exhibit good precision; and that the colors of the reagent pads are independent of operator technique, sample volume (20-50 microL), and effects of potential interferents studied (although high concentrations of fluoride slightly inhibited color development). Glucose measurements obtained visually with the Visidex system correlated well with values obtained with a YSI Glucose Analyzer (for two separate studies, slope = 0.96 and 1.04, r = 0.99 and 0.96, and n = 172 and 543, respectively).

scholarly journals Determination of Zeranol and its Metabolites in Bovine Muscle Tissue with Gas Chromatography-Mass Spectrometry

2012 ◽  
Vol 56 (3) ◽  
pp. 335-342 ◽  
Author(s):  
Iwona Matraszek-Żuchowska ◽  
Barbara Woźniak ◽  
Jan Żmudzki
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Muscle Tissue ◽  
Solid Phase ◽  
Performance Criteria ◽  
Gas Chromatography Mass Spectrometry ◽  
The European Union ◽  
Bovine Muscle ◽  
Chromatography Mass Spectrometry

Abstract This paper describes the quantitative method of determination of chosen substances from resorcylic acid lactones group: zeranol, taleranol, α-zearalenol, β-zearalenol, and zearalanone in bovine muscle tissue. The presented method is based on double diethyl ether liquid-liquid extraction (LLE), solid phase extraction (SPE) clean up, and gas chromatography mass spectrometry (GC-MS) analysis. The residues were derivatised with a mixture of N-methyl-N-trimethylsilyltrifluoroacetamide, ammonium iodide, and DL-dithiothreitol (1,000:2:5, v/w/w). The GC-MS apparatus was operated in positive electron ionisation mode. The method was validated according to the European Union performance criteria pointed in Decision Commission 2002/657/EC. The average recoveries of all analytes at 1 μg kg-1 level were located between 83.7% and 94.5% values with the coefficients of variation values <25%. The decision limits (CCα) and detection capabilities (CCβ) for all analytes ranged from 0.58 to 0.82 μg kg-1 and from 0.64 to 0.94 μg kg-1, respectively. The procedure has been accredited and is used as a screening and confirmatory method in control of hormone residues in animal tissues.

scholarly journals Multimycotoxin Analysis by LC-MS/MS in Cereal Food and Feed: Comparison of Different Approaches for Extraction, Purification, and Calibration

2018 ◽  
Vol 101 (3) ◽  
pp. 647-657 ◽  
Author(s):  
Michele Solfrizzo ◽  
Lucia Gambacorta ◽  
Rita Bibi ◽  
Martina Ciriaci ◽  
Angela Paoloni ◽  
...  
Keyword(s):  
Matrix Effects ◽  
Solid Phase ◽  
Tandem Ms ◽  
Proficiency Tests ◽  
Food And Feed ◽  
Z Scores ◽  
High Matrix ◽  
Extraction Solvents ◽  
Lc Tandem Ms

Abstract Twelve different approaches commonly used for the simultaneous LC tandem MS (MS/MS) determination of mycotoxins (deoxynivalenol, aflatoxins, ochratoxin A, T-2 and HT-2 toxins, fumonisins, and zearalenone) were tested in cereals and feed materials. They comprised different extraction solvents, types of cleanup [solid-phase extraction, QuEChERS, and immunoaffinity (IMA)], and calibration approaches (external or matrix-matched). The percentage of mycotoxins with acceptable recovery, according to Regulation (EC) No. 401/2006, ranged from 9 to 100%. The approach giving the highest percentage of acceptable results was selected and further tested for corn, rice, and feed spiked at three different mycotoxin levels (low, medium, and high). The method is based on extraction with MeOH–water (70 + 30, v/v) and cleanup with two multiantibody IMA columns. For corn and rice spiked at low mycotoxin levels, a significant matrix effect was observed and was compensated by using 13C calibration. At higher mycotoxin levels (medium and high), matrix effects were negligible as no significant differences were observed for the majority of recovery results calculated by 13C calibration and external calibration. Although the proposed method still needs improvement in terms of accuracy and, to a lesser extent, precision, it was successfully tested with four proficiency tests in buckwheat, corn, rice, and feed, giving acceptable z-scores for 97% (34 out of 35) of results.

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 Determination of Organophosphorus Pesticide Residues in Milk

2013 ◽  
Vol 57 (2) ◽  
pp. 185-189 ◽  
Author(s):  
Tomasz Kiljanek ◽  
Alicja Niewiadowska ◽  
Stanisław Semeniuk
Keyword(s):  
Pesticide Residues ◽  
Solid Phase ◽  
Organophosphorus Pesticides ◽  
Organophosphorus Pesticide ◽  
Gel Permeation Chromatography ◽  
Proficiency Tests ◽  
The European Union ◽  
Photometric Detection ◽  
Milk Samples

Abstract A method for simultaneous determination of 13 organophosphorus pesticide residues in milk samples has been developed and validated. The method is based on the extraction of the sample with acetone and petroleum ether, cleanup by gel permeation chromatography, and solid phase extraction, and determination by gas chromatography with flame photometric detection. The recovery, investigated by analysing blank milk samples spiked with azinphos, chlorfenvinphos, chlorpyrifos, chlorpyrifos-methyl, diazinon, fenitrothion, methacrifos, methidathion, parathion-methyl, pyrazophos, and triazophos at concentrations of 10, 20, and 30 μg/kg, and with parathion and pirimiphos-methyl at concentrations of 25, 50, and 75 μg/kg, ranged from 73.1% to 106.2%. Performance characteristics, such as repeatability and within-laboratory reproducibility expressed as coefficient of variation were less than 20%. Measurement uncertainty was lower than 22% for all validated organophosphorus pesticides. The limits of quantification were 10 μg/kg for all compounds and allowed determination of residues at, or even below, the maximum residue limits set by the European Union. The satisfactory z-score results of international proficiency tests confirm good accuracy, reproducibility, and reliability of the developed method.

scholarly journals Sensitive Sandwich Enzyme Immunoassay for Serum Ferritin on Microtitre Plates

1981 ◽  
Vol 18 (1) ◽  
pp. 48-53 ◽  
Author(s):  
Sukanya Linpisarn ◽  
Larry J Kricka ◽  
John H Kennedy ◽  
Thomas P Whitehead
Keyword(s):  
Enzyme Immunoassay ◽  
Serum Ferritin ◽  
Clinical Laboratory ◽  
Solid Phase ◽  
Good Precision ◽  
Ferritin Concentration ◽  
Assay Procedure ◽  
Serum Ferritin Concentration ◽  
Sandwich Enzyme Immunoassay

A solid-phase sandwich enzyme immunoassay for serum ferritin is described. The assay procedure was simple, showed good precision, and was suitable for the routine determination of serum ferritin concentration in a clinical laboratory. The assay compared well with a conventional radioimmunoassay for ferritin. The assay was extremely sensitive and had a detection limit of 2·2 pg.

scholarly journals Development and Validation of a HPLC-UV Method for Simultaneous Determination of Five Sulfonylurea Herbicide Residues in Groundnut Oil Followed by Matrix Solid-Phase Dispersion

2012 ◽  
Vol 2012 ◽  
pp. 1-5 ◽  
Author(s):  
T. Nageswara Rao ◽  
A. Ramesh ◽  
T. Parvathamma
Keyword(s):  
Ethyl Acetate ◽  
High Performance ◽  
Solid Phase ◽  
Sulfonylurea Herbicide ◽  
Groundnut Oil ◽  
Herbicide Residues ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard

A simple, sensitive, and inexpensive method was developed using matrix solid-phase dispersion (MSPD), together with high performance liquid chromatographic method for determination of sulfonylurea herbicide residues (nicosulfuron, pyrazosulfuron ethyl, metsulfuron methyl, chlorsulfuron and azimsulfuron) in groundnut oil. The evaluated parameters included the type and amount of sorbent (silica gel, C 18 and florisil) and the nature of eluent (ethyl acetate, dichloromethane, and acetonitrile). The best results were obtained using 1.0 g of groundnut oil sample, 1.0 g of C 18 as sorbent, and 20 mL of ethyl acetate-dichloromethane (1 : 1, (v/v)). The method was validated using groundnut oil samples spiked with sulfonylurea herbicides at different concentration levels (0.05 and 0.5 g/mL). Average recoveries (using each concentration six replicates) ranged 90–97%, with relative standard deviations less than 3%, the concentration of calibration solutions was in the range 0.01–2.0 g/mL and limits of detection (LOD) as well as limits of quantification (LOQ) were 0.01 g/mL and 0.05 g/mL, respectively.

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