scholarly journals Determination of patulin in apple juice by liquid chromatography-electrospray tandem mass spectrometry

2021 ◽  
Vol 854 (1) ◽  
pp. 012075
Author(s):  
T Radicevic ◽  
S Jankovic ◽  
S Simunovic ◽  
S Stefanovic ◽  
Z Petrovic ◽  
...  
Keyword(s):  
Apple Juice ◽  
Limit Of Detection ◽  
Fruit Juices ◽  
Human Consumption ◽  
Human Diet ◽  
Maximum Residue Limits ◽  
Commission Regulation ◽  
Apple Products ◽  
Infants And Young Children

Abstract Patulin is a mycotoxin produced by several fungi, (Penicillium, Aspergillus, Byssochlamys). The main sources of patulin intake in human diet are apples, apple juice and apple nectar, and for this reason, apple based foods are monitored for the presence of this mycotoxin. Commission Regulation EC No 1881/2006 lays down maximum residue limits (MRLs) of 50 µg/kg in apple juice and cider, 25 µg/kg in solid apple products, and 10 µg/kg in products for infants and young children. In Serbia, maximum permitted amounts of patulin in fruit juices, reconstituted concentrated fruit juices and fruit nectars, as well as in solid apple products, including apple compote and apple puree, intended for direct human consumption are prescribed in the Regulation on maximum concentrations of certain contaminants in foodstuffs. This paper presents the LC-MS/MS method for quantitative determination of patulin in apple juice. Criteria for method validation were taken from Commission Decision 2002/657/EC. Linearity was confirmed in the concentration ranges of 0-100 µg/kg, with the limit of detection (LoD) of 9.85 µg/kg. The performance of the method was successfully verified by participating in a proficiency study.

Capillary Gas Chromatographic Determination of Thiabendazole in Citrus and Apple Juices

1994 ◽  
Vol 77 (5) ◽  
pp. 1293-1296 ◽  
Author(s):  
Mitsuo Oishi ◽  
Kazuo Onishi ◽  
Itsu Kano ◽  
Hiroyuki Nakazawa ◽  
Shinzo Tanabe
Keyword(s):  
Limit Of Detection ◽  
Simple Procedure ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Fruit Juices ◽  
Reduced Pressure ◽  
Standard Solution ◽  
Juice Sample ◽  
Nitrogen Phosphorus

Abstract A rapid and simple procedure for the determination of thiabendazole (TBZ) residue in citrus and apple juices is described. A juice sample is made basic with 2M NaOH and applied to a disposable Extrelut prepacked column. TBZ is eluted with hexane–ethyl acetate (3 + 1) from the column. The eluate is evaporated to dryness under reduced pressure and then dissolved in an internal standard solution. TBZ is monitored without derivatization by capillary gas chromatography with nitrogen-phosphorus detection. The recoveries of TBZ added to fruit juices at 0.05-1.0 μg/g were 90-96%. The limit of detection of the method for TBZ was 0.01 μg/g. The proposed method is rapid, simple, and sensitive and is applicable to the determination of TBZ in commercial fruit juices.

scholarly journals Residues of Chlormequat and Mepiquat in Grain—Results from the Danish National Pesticide Survey

1999 ◽  
Vol 82 (2) ◽  
pp. 331-336 ◽  
Author(s):  
René K Juhler ◽  
Martin Vahl
Keyword(s):  
Limit Of Detection ◽  
Internal Standard ◽  
Mass Spectrometric ◽  
Human Consumption ◽  
Tandem Mass ◽  
Internal Standards ◽  
Limit Of Determination ◽  
Maximum Residue Limits ◽  
Tandem Mass Spectrometric ◽  
Liquid Chromatographic

Abstract The objective of the present work was to establish information on chlormequat and mepiquat residues in grain for human consumption. Chlormequat (2- chloro-N,N,N-trimethylethylammonium, CAS RN 7003-89-6) and mepiquat (1,1-dimethylpiperid- inium, CAS RN 15302-91-7) are plant growth regulators used to stabilize stalks in cereals. The study was part of the Danish National Pesticide Survey, managed by the Danish Veterinary and Food Administration. Samples were collected in autumn 1997. Residue contents were determined with a newly developed liquid chromatographic- tandem mass spectrometric (LC-MS/MS) method for chlormequat analysis. The method was extended to include mepiquat in the present study. Quantitation was done by the internal standards method, using mass chromatograms of the most intense daughter ions of mepiquat (m/z 98), chlormequat (m/z 58), and [13C]-chlormequat (m/z 61, internal standard). For chlormequat, the overall limit of detection (LD) was 6 μg/kg and the limit of determination (LOD) was 10 μg/kg. For mepiquat, LD was 2 μg/kg and LOD was 3 μg/kg. Of 77 samples analyzed, 51 contained chlormequat and 11 contained mepiquat. The highest levels of chlormequat were found in samples of oatmeal (3.76 mg/kg) and rye (1.08 mg/kg). In 9 rye grain samples containing chlormequat, 5 also contained mepiquat. However, in all samples analyzed, the residues of chlormequat and mepiquat were below maximum residue limits.

scholarly journals Determination of Dialkyl Phosphates as Breakdown Products of Organophosphorus Insecticides in Fruit Juices by HPTLC with Fluorescence Detection

2009 ◽  
Vol 92 (3) ◽  
pp. 691-698 ◽  
Author(s):  
Wolfgang Schwack ◽  
Tatjana Zeisler ◽  
Constanze Stiefel
Keyword(s):  
Apple Juice ◽  
Degradation Products ◽  
Organophosphorus Pesticides ◽  
Internal Standard ◽  
Barium Chloride ◽  
Fruit Juices ◽  
Limit Of Quantification ◽  
Dimethyl Phosphate ◽  
Relative Standard

Abstract Dialkyl phosphates (DAP) are common degradation products of organophosphorus pesticides that are used as urinary biomarkers for human exposure. An HPTLC method was developed for the quantitative determination of DAP in fruit juices, i.e., dimethyl phosphate (DMP), dimethyl thiophosphate (DMTP), diethyl phosphate (DEP), and diethyl thiophosphate (DETP). Dibutyl phosphate (DBP) was used as an internal standard. The method was based on precipitation of fruit acids in the presence of barium chloride and acetonitrile and liquidliquid extraction with acetonitrilediethyl ether. Extracted DAP were derivatized with 1-(bromoacetyl)pyrene (BAP), and the BAP derivatives separated on HPTLC amino plates with dichloromethane as the mobile phase. Densitometry was performed by measurement of fluorescence at 366/>400 nm. The limit of quantification (LOQ) values were between 0.8 and 1.4 ng/zone. Fluorescence enhancement was achieved by dipping the plate into a paraffin oil solution, increasing the sensitivity and resulting in an LOQ of 0.50.6 ng/zone. Repeatabilities with relative standard deviations of 3.5 (n = 5, at 1520 ng/zone) and coefficients of correlation of 0.9999 were highly satisfactory for rapid trace analysis of DAP in the fruit juices by HPTLC. The mean recoveries from apple juice spiked at 0.5 mg/L were 74, 83, 70, and 57 for DMP, DEP, DMTP, and DETP, respectively. If an application volume of 5 L of apple juice extract was applied, the LOQ in apple juice was 300 g/L. However, this can be lowered by application of higher volumes (up to 50 L) or a more concentrated derivatization batch.

Anodic Adsorptive Stripping Voltammetric Determination of Rafoxanide on Glassy Carbon Electrode

2020 ◽  
Vol 23 (10) ◽  
pp. 1002-1009
Author(s):  
Abd-Elgawad Radi ◽  
Hassan El-samboskany
Keyword(s):  
Glassy Carbon ◽  
Fasciola Hepatica ◽  
Limit Of Detection ◽  
Bovine Milk ◽  
Active Agent ◽  
Human Consumption ◽  
Irreversible Adsorption ◽  
Simple Method ◽  
Ph Range

Background: Rafoxanide (RFX) is an active agent against Fasciola hepatica, but it is prohibited for treatment of dairy animals whose milk is provided for human consumption. Objective: A reliable, fast, and simple method needs to be developed to monitor RFX residues in milk samples before distribution to consumers. Methods: In this work, the electrochemical oxidation of RFX was studied at glassy carbon electrodes (GCE) in Britton-Robinson buffer (BR) solutions over the pH range 2.0-12.0 using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The oxidation of the drug was accomplished in a single irreversible, adsorption-controlled step within the pH range 4.0-9.0. Therefore, the application of GCE for a sensitive and selective quantification of RFX by adsorptive stripping voltammetry was reported. The accumulation of the analyte was performed in Britton–Robinson buffer (pH 5.0) at a potential of -0.3 V (vs. Ag-AgCl-KClsat) for 300 s and the measurement was carried out, after medium exchange, in BR solution of pH 7.0 using DPV. Result and Conclusion: This format was satisfactorily applied for the determination of RFX in bovine milk. Limit of detection (LOD) of 1.25 µg kg -1 of milk and mean recoveries of 97.8 to 107.5% were achieved.

scholarly journals Single-Laboratory Validation of a Method for the Determination of Furan in Foods by Using Static Headspace Sampling and Gas Chromatography/Mass Spectrometry

2006 ◽  
Vol 89 (5) ◽  
pp. 1417-1424 ◽  
Author(s):  
Patricia J Nyman ◽  
Kim M Morehouse ◽  
Timothy P McNeal ◽  
Gracia A Perfetti ◽  
Gregory W Diachenko
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Apple Juice ◽  
Limit Of Detection ◽  
Peanut Butter ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract A headspace gas chromatography/mass spectrometry method was developed and validated in-house for the determination of furan in foods. The method of standard additions with d4-furan as the internal standard was used to quantitate furan. The limit of detection and limit of quantitation (LOQ) values ranged from 0.2 and 0.6 ng/g, respectively, in apple juice to 0.9 and 2.9 ng/g, respectively, in peanut butter. Recoveries were obtained at 0.5, 1, 2, and 3 times the LOQ. At 1, 2, and 3 times the LOQ, the recoveries ranged from 89.4 to 108%, and the relative standard deviations ranged from 3.3 to 17.3% for all the matrixes. For apple juice, chicken broth, and infant formula, the averaged coefficients of determination from the linear regression analyses were >0.99 with each food fortified at 0.5, 1, 2, and 3 times the LOQ. The coefficients of determination were >0.99 for green beans and 0.96 for peanut butter with the foods fortified at 1, 2, and 3 times the LOQ. Within-laboratory precision was determined by comparing the amounts of furan found in 18 samples by 2 analysts on different days with different instruments. For most of the foods, the difference between the amounts found by each analyst was <18%. The method was used to conduct a survey of >300 foods. The furan levels found ranged from none detected to 174 ng/g.

scholarly journals Comparison of detection sensitivity of five microbial inhibition tests for the screening of aminoglycoside residues in fortified milk

2012 ◽  
Vol 30 (No. 4) ◽  
pp. 314-320 ◽  
Author(s):  
Z. Sýkorová Goffová ◽  
I. Kožárová ◽  
D. Máté ◽  
S. Marcinčák ◽  
Z. Gondová ◽  
...  
Keyword(s):  
Bacillus Stearothermophilus ◽  
Test Strain ◽  
Detection Sensitivity ◽  
Antibiotic Residues ◽  
Milk Samples ◽  
Microbial Inhibition ◽  
Fortified Milk ◽  
Maximum Residue Limits ◽  
Commission Regulation

The assessment of detection sensitivity of five microbial inhibition tests (MITs), STAR (screening test for antibiotic residues) with the test strain Bacillus subtilis BGA, Delvotest<sup>&reg; </sup>S&nbsp; P-NT, Total Antibiotics, Kalidos TB, and Kalidos MP with the test strain Bacillus stearothermophilus var. calidolactis to five aminoglycosides (AMGs), gentamicin, neomycin, streptomycin, kanamycin, and spectinomycin in fortified milk samples were studied. The sensitivity of MITs to AMGs was evaluated on the basis of experimental determination of detection limits (LODs) of MITs for AMGs. The LODs of these tests were compared with the maximum residue limits (MRLs) established for milk by the Commission Regulation (EU) No. 37/2010. LODs of STAR for AMGs in fortified milk samples were at the levels of MRL for neomycin (1.50 &micro;g/g), gentamicin (0.10&nbsp;&micro;g/g), streptomycin (0.20 &micro;g/g) and kanamycin (0.15 &micro;g/g). Spectinomycin (0.20 &micro;g/g) was not detected at the level of MRL. The LODs determined by Delvotest<sup>&reg; </sup>SP-NT, Total Antibiotics and Kalidos MP were comparable, but only gentamicin and neomycin were reliably detected at the levels of MRL. Kalidos TB was more sensitive to AMGs than Delvotest<sup>&reg; </sup>SP-NT, Total Antibiotics and Kalidos MP. Gentamicin, neomycin and streptomycin were detected at the levels of MRL. &nbsp;

scholarly journals Electrochemical Sensor Based on a Carbon Veil Modified by Phytosynthesized Gold Nanoparticles for Determination of Ascorbic Acid

Sensors ◽  
2020 ◽  
Vol 20 (6) ◽  
pp. 1800 ◽  
Author(s):  
Khiena Z. Brainina ◽  
Maria A. Bukharinova ◽  
Natalia Yu. Stozhko ◽  
Sergey V. Sokolkov ◽  
Aleksey V. Tarasov ◽  
...  
Keyword(s):  
Gold Nanoparticles ◽  
Ascorbic Acid ◽  
Limit Of Detection ◽  
Fruit Juices ◽  
Optimal Parameters ◽  
X Ray ◽  
Titration Data ◽  
Higher Sensitivity ◽  
Good Agreement

An original voltammetric sensor (Au-gr/CVE) based on a carbon veil (CV) and phytosynthesized gold nanoparticles (Au-gr) was developed for ascorbic acid (AA) determination. Extract from strawberry leaves was used as source of antioxidants (reducers) for Au-gr phytosynthesis. The sensor was characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy and electrochemical methods. Optimal parameters of AA determination were chosen. The sensor exhibits a linear response to AA in a wide concentration range (1 μM–5.75 mM) and a limit of detection of 0.05 μM. The developed sensor demonstrated a high intra-day repeatability of 1 μM AA response (RSD = 1.4%) and its stability during six weeks, selectivity of AA determination toward glucose, sucrose, fructose, citric, tartaric and malic acids. The proposed sensor based on Au-gr provides a higher sensitivity and a lower limit of AA detection in comparison with the sensor based on gold nanoparticles synthesized by the Turkevich method. The sensor was successfully applied for the determination of AA content in fruit juices without samples preparation. The recovery of 99%–111% and RSD no more than 6.8% confirm the good reproducibility of the juice analysis results. A good agreement with the potentiometric titration data was obtained. A correlation (r = 0.9867) between the results of AA determination obtained on the developed sensor and integral antioxidant activity of fruit juices was observed.

scholarly journals Categorization of animal by-products and labelling of derived products with of glycerol triheptanoate (GTH)

2019 ◽  
Vol 75 (05) ◽  
pp. 6250-2019
Author(s):  
ALEKSANDRA GRELIK ◽  
EWELINA KOWALCZYK ◽  
KRZYSZTOF KWIATEK
Keyword(s):  
Animal Health ◽  
Control Measures ◽  
Animal Origin ◽  
Human Consumption ◽  
Mass Spectrometry Detection ◽  
Processing Plants ◽  
Commission Regulation ◽  
Rendered Fat ◽  
By Products

Animal by-products result mainly from the slaughter of animals for human consumption, the production of products of animal origin (such as dairy products), the disposal of dead animals, and disease-control measures. Regardless of their source, they pose a potential risk to public and animal health and the environment. This risk needs to be adequately controlled, either by safe disposal of such products, or by their utilization, provided that strict conditions are maintained to minimize the health risks involved. Animal by-products are classified into categories that reflect the level of risk to public and animal health arising from those by-products (Cat. 1, 2 and 3). According to Commission Regulation (EU) No 142/2011, in processing plants for the processing of Category 1 or 2 material, derived products shall be permanently marked with glycerol triheptanoate (GTH). The minimum content of marker in target materials is 250 mg/kg of fat. For the determination of glycerol triheptanoate in dry meat, bone meals, rendered fat and soil adjuvants, gas chromatography technique and mass spectrometry detection are used

SERUM TRIIODOTHYRONINE DETERMINATION BY SATURATION ANALYSIS

1973 ◽  
Vol 72 (4) ◽  
pp. 714-726 ◽  
Author(s):  
A. Burger ◽  
B. Miller ◽  
C. Sakoloff ◽  
M. B. Vallotton
Keyword(s):  
Ionic Strength ◽  
Limit Of Detection ◽  
Improved Method ◽  
Accuracy Of Measurement ◽  
Tracer Amount ◽  
The Mean ◽  
Physiological Values ◽  
Hyperthyroid Patients ◽  
Solvent Blank

ABSTRACT An improved method for the determination of serum triiodothyronine (T3) has been developed. After addition of a tracer amount of the hormone, T3 was extracted from 1 ml serum under conditions of pH and ionic strength which favoured T3 extraction (89%) over thyroxine (T4) extraction (58%). Chromatography of the extracted material on Sephadex LH-20 separated T3 completely from residual T4. The T3 eluate was dried, then re-dissolved in 0.5 ml NaOH 0.04 n. To 0.2 ml duplicate aliquots, a standard amount of TBG was added for the competitive protein analysis. After one hour incubation at 4°C, separation of bound from free T3 was achieved on small Sephadex G-25 columns. Overall recovery was 67 ± 10.8% and correction for the loss was made. The solvent blank was 37 ± 27 (sd) ng/100 ml. Accuracy of measurement of known quantities of T3 added to serum was 98.4%. The coefficient of variation within the assay was 6.2% and between the assays it was 11.4%. The limit of detection (0.1 ng) corresponded to a concentration of 25 ng/100 ml. T4 added to serum did not interfere with T3 determination until high non-physiological values were reached. The mean ± sd serum T3 in 54 euthyroid subjects was 153 ± 58 ng/100 ml and in 24 hyperthyroid patients it was 428 ±186 ng/100 ml; 4 out of the 24 hyperthyroid values were within 2 sd of the mean euthyroid group. All the values found in the euthyroid group were well above the limit of detection of the method.

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