scholarly journals A Targeted UHPLC-MS/MS Method Validated for the Quantification of Ergot Alkaloids in Cereal-Based Baby Food from the Belgian Market

Toxins ◽  
2021 ◽  
Vol 13 (8) ◽  
pp. 531
Author(s):  
Bart Huybrechts ◽  
Svetlana V. Malysheva ◽  
Julien Masquelier
Keyword(s):  
Ergot Alkaloid ◽  
Ergot Alkaloids ◽  
Residue Level ◽  
Baby Food ◽  
Good Sensitivity ◽  
The European Union ◽  
Modified Quechers ◽  
Maximum Residue Level ◽  
Accuracy And Precision ◽  
Sample Testing

Following pending new legislation in the European Union setting a maximum of 20 ng g−1 for the total sum of ergot alkaloids in dry cereal-based baby food, a new UHPLC-MS/MS method was developed. It is suitable for the quantification of six ergot alkaloids: Ergocornine, ergocristine, ergometrine, ergosine, ergotamine, α-ergocryptine, and their corresponding epimers. The method is able to reliably detect individual ergot alkaloids at a level as low as 0.5 ng g−1. The method uses a modified QuEChERS extraction approach before UHPLC-MS/MS analysis. The method showed good sensitivity, accuracy, and precision. It has been applied to 49 samples from the Belgian market. In 26 samples, not a single ergot alkaloid was detected while in 23 out of 49 samples at least one ergot alkaloid was detected with 2 samples containing 12 ergot alkaloids. Ergometrine was the alkaloid most frequently detected i.e., 16 out of 49 samples. Only one sample, testing positive for all 12 ergot alkaloids, would be non-conforming to the newly proposed Maximum Residue Level (MRL).

scholarly journals The development of methods for the determination of residues of the insecticide pymetrozine in water, soil, cucumber and rape

2019 ◽  
pp. 79-87
Author(s):  
Mikhail F. Zayats ◽  
Sergey M. Leschev
Keyword(s):  
Experimental Data ◽  
Orthophosphoric Acid ◽  
Residue Level ◽  
Inorganic Salts ◽  
Diode Array ◽  
The European Union ◽  
Optimal Conditions ◽  
Ultraviolet Detection ◽  
Maximum Residue Level

Based on the literature data on the solubility of pymetrozine in water and organic solvents, as well as experimental data on the extraction of pymetrozine from water, soil and plant matrices, the optimal conditions for the extraction of pymetrozine from water; soil; cucumber; rape seeds, oil and green pods were selected. The conditions for cleaning extracts were selected as well. At the first stage, acetonitrile, a mixture of dichloromethane – isopropanol, or a mixture of dichloromethane – methanol in the presence or absence of inorganic salts were used for extraction of the pesticide. Pymetrozine was found to be a highly hydrophilic substance. For the purification of extracts of pymetrozine from plant matrices the extraction systems hexane – 0.02 mol/L aqueous solution of orthophosphoric acid, hexane or chloroform – aqueous solutions of ammonium sulfate were successfully used. The samples, obtained after this treatment, were pure enough to determine the residual amounts of pymetrozine in them at the maximum residue level (MRL), determined in Russia and the countries of the European Union, or lower using widespread liquid chromatography with diode-array (ultraviolet) detection.

scholarly journals Assessment of ergot (Claviceps purpurea) exposure in pregnant and postpartum beef cows

2018 ◽  
Vol 98 (4) ◽  
pp. 688-700 ◽  
Author(s):  
T. Grusie ◽  
V. Cowan ◽  
J. Singh ◽  
J. McKinnon ◽  
B. Blakley
Keyword(s):  
Ergot Alkaloid ◽  
Post Partum ◽  
Ergot Alkaloids ◽  
Maximum Size ◽  
Beef Cows ◽  
Plasma Prolactin ◽  
Claviceps Purpurea ◽  
Ambient Temperatures ◽  
Beef Cow ◽  
The Impact

Cows were fed ration for 9 wk containing 5, 48, 201, and 822 μg kg−1 ergot alkaloids. The objective was to evaluate the impact of ergot consumption in beef cow–calf operations. Ergot alkaloids up to 822 μg kg−1 did not alter the weight of peripartum and postpartum beef cows (P = 0.93) or nursing calves (P = 0.08), rectal temperature (P = 0.16), or plasma prolactin concentrations (P = 0.30) at moderate ambient temperatures. Ergot did not influence the time (>1 ng mL−1; P = 0.79) or the progesterone concentration (P = 0.38) at the time of first postpartum rise or the size of the first (14 ± 0.6 mm; P = 0.40) and second (13 ± 0.5 mm; P = 0.41) follicles to ovulate. The maximum size of the first postpartum corpus luteum (CL) was 4 mm larger in the 822 μg kg−1 ergot group compared with the control (P = 0.03) for the first ovulation post partum, but not for the second (P = 0.11). There was no effect of ergot exposure on the number of days until the appearance of the first (43 ± 4 d; P = 0.95) or second (52 ± 4 d; P = 0.98) CL post partum. Ergot alkaloid concentrations up to 822 μg kg−1 did not affect pregnancy rates (X2 = 0.36). In conclusion, ergot alkaloid exposure for 9 wk to concentrations as high as 822 μg kg−1 did not alter performance in pregnant and postpartum beef cattle at moderate ambient temperatures.

Isolation of ergovaline, ergoptine, and ergonine, new alkaloids of the peptide type, from ergot sclerotia

1979 ◽  
Vol 57 (13) ◽  
pp. 1638-1641 ◽  
Author(s):  
Rudolf Brunner ◽  
Peter Leopold Stütz ◽  
Hans Tscherter ◽  
Paul Albert Stadler
Keyword(s):  
Total Synthesis ◽  
Ergot Alkaloid ◽  
Ergot Alkaloids ◽  
Extraction Processes

The isolation of three new ergot alkaloids of the peptide type from sclerotia of Clavicepspurpurea and from mother liquors of rye ergot alkaloid extraction processes is described. The constitution of the new alkaloids ergovaline, ergoptine, and ergonine has been established by comparison with compounds previously obtained by total synthesis.

PENENTUAN KADAR RESIDU TETRASIKLIN HCl PADA IKAN AIR TAWAR YANG BEREDAR DI PASAR SEGIRI MENGGUNAKAN METODE SPEKTROFOTOMETRI ULTRA VIOLET

2017 ◽  
Vol 2 (2) ◽  
pp. 173
Author(s):  
Henny Nurhasnawati ◽  
Siti Jubaidah ◽  
Novita Elfia
Keyword(s):  
Freshwater Fish ◽  
Ultra Violet ◽  
Standard Addition ◽  
Fish Farming ◽  
Residue Level ◽  
Ultraviolet Spectrophotometry ◽  
Maximum Residue Level ◽  
Traditional Market ◽  
Antibiotic Residue ◽  
Tetracycline Hcl

Tetracycline HCl is one of the most commonly used antibiotics in fish farming that aims to control diseases caused by bacteria. The purpose of this study was to determine the presence and the level of tetracycline HCl antibiotic residue in freshwater fishes sold at the Segiri traditional market. The method used in this research was a standard addition ultraviolet spectrophotometry. The results showed that residue level of tetracycline HCl in freshwater fish is 192,067 μg/g – 257,409 μg/g. These result was far exceeded the maximum residue level of tetracycline class antibiotics in meat and dairy based on SNI 01-6366-2000 that limit the residue not higher than 0.1 μg/g

scholarly journals Modification of the existing maximum residue level for ethephon in kaki/Japanese persimmons

EFSA Journal ◽  
2017 ◽  
Vol 15 (3) ◽  
Author(s):  
◽  
Alba Brancato ◽  
Daniela Brocca ◽  
Chloé De Lentdecker ◽  
Zoltan Erdos ◽  
...  
Keyword(s):  
Residue Level ◽  
Maximum Residue Level

scholarly journals Deltamethrin residues applied in different formulations in staked cucumber and the actions of insecticides on the pickleworm control

2008 ◽  
Vol 26 (3) ◽  
pp. 321-324 ◽  
Author(s):  
Gilberto C de Baptista ◽  
Luiz Roberto P Trevizan ◽  
André A Franco ◽  
Renato A da Silva
Keyword(s):  
Gas Chromatography ◽  
Pesticide Residues ◽  
Residue Level ◽  
Concentrate Suspension ◽  
Evaluation Period ◽  
Emulsifiable Concentrate ◽  
Maximum Residue Level ◽  
Low Levels ◽  
Vegetables And Fruits ◽  
Sampling Times

Pesticide residues, especially in vegetables and fruits, are a reason for concern with respect to the health of consumers and workers that need to return to areas that have been treated with these agrochemicals. The objectives of this experiment were to (a) study the behavior of deltamethrin residues from different formulations on cucumber fruits; and (b) correlate insecticide contents in the fruits with pickleworm control. Treatments were as follows: (a) control; (b) three 30 mL applications of deltamethrin 25 EC 100 L-1 water (emulsifiable concentrate formulation); (c) three 7.5 mL applications of deltamethrin 100 EC 100 L-1 water (emulsifiable concentrate); and (d) three 3.75 mL applications of deltamethrin 200 CS 100 L-1 water (concentrate suspension). Samples were taken at (-1), zero, 1; 3; 5; 7, and 14 days after the last application. Residues were determined by the gas chromatography technique, using an electron capture detector. In order to evaluate insecticide effectiveness, six infestation surveys were conducted during the same sampling times. Although at low levels, the deltamethrin residues in the fruits were above the maximum residue level (MRL = 0.03 mg kg-1), even one day after the end of the safety interval (2 days), and were higher for the CS formulation. The insecticide was effective to control the pest during the entire evaluation period.

Rate of decrease of the residual concentration of diazinon in cabbage

1980 ◽  
Vol 20 (105) ◽  
pp. 504
Author(s):  
JR Hargreaves ◽  
KJ Melksham
Keyword(s):  
Initial Period ◽  
Residue Level ◽  
Spray Application ◽  
Rapid Decay ◽  
Residual Concentration ◽  
First Order ◽  
First Order Kinetics ◽  
Maximum Residue Level

Analysis of diazinon residues in cabbages up to 14 days after the final spray application, showed an initial period of rapid decay followed by a period of slower decay, which approximates to first order kinetics. The Australian maximum residue level of 0.7 mg kg-1 diazinon for the whole cabbage was reached in 2-3 days in summer and 7-8 days in winter. The recommended Australia 14-day withholding period, combined with marketing of hearts alone, conformed to Japanese marketing requirements of 0.1 mg kg-1.

scholarly journals Influence of Prolonged Serotonin and Ergovaline Pre-Exposure on Vasoconstriction Ex Vivo

Toxins ◽  
2021 ◽  
Vol 14 (1) ◽  
pp. 9
Author(s):  
Eriton E. L. Valente ◽  
David L. Harmon ◽  
James L. Klotz
Keyword(s):  
Blood Vessels ◽  
Ergot Alkaloid ◽  
Inhibitory Concentration ◽  
Contractile Response ◽  
Ex Vivo ◽  
Ergot Alkaloids ◽  
Exposure Period ◽  
Inhibitory Response ◽  
Previous Exposure ◽  
Ic50 Concentration

Ergot alkaloid mycotoxins interfere in many functions associated with serotonergic neurotransmitters. Therefore, the objective was to evaluate whether the association of serotonin (5-hydroxytryptamine, 5-HT) and ergot alkaloids during a 24 h pre-incubation could affect the vascular contractile response to ergot alkaloids. To evaluate the effects of 24 h exposure to 5-HT and ergot alkaloids (ergovaline, ERV), two assays were conducted. The first assay determined the half-maximal inhibitory concentration (IC50) following the 24 h pre-exposure period, while the second assay evaluated the effect of IC50 concentrations of 5-HT and ERV either individually or in combination. There was an interaction between previous exposure to 5-HT and ERV. Previous exposure to 5-HT at the IC50 concentration of 7.57 × 10−7 M reduced the contractile response by more than 50% of control, while the exposure to ERV at IC50 dose of 1.57 × 10−10 M tended to decrease (p = 0.081) vessel contractility with a response higher than 50% of control. The 24 h previous exposure to both 5-HT and ERV did not potentiate the inhibitory response of blood vessels in comparison with incubation with each compound alone. These results suggest receptor competition between 5-HT and ERV. More studies are necessary to determine the potential of 5-HT to treat toxicosis caused by ergot alkaloids.

scholarly journals The Political Economy of Standards: Does MRLs Matter in Cottonseed and its Trade?

2017 ◽  
Vol II (I) ◽  
pp. 177-196
Keyword(s):  
Cottonseed Oil ◽  
Ordinary Least Squares ◽  
Residue Level ◽  
International Standards ◽  
The Political ◽  
Maximum Residue Limit ◽  
Maximum Residue Level ◽  
Maximum Residue Limits ◽  
Regression Estimators ◽  
Crude Cottonseed Oil

In this paper, we introduce three indices of trade which are consequently applied to the case maximum residue level, MRLs of pesticide. The aggregation indices of NTM i.e Li and Beghin index of trade, Heterogeneous index of trade (HIT) and actual heterogeneous index of trade (AHIT) regulations to compute their protectionism relative to international standards. The application of indices to Maximum Residue Limit (MRL) affecting cottonseed and its by-product i.e crude cottonseed oil and refined cottonseed oil, using a science-based standards Codex Alimentarius. In this analysis, the main aim of the article is to show the response of the maximum residue limits (MRLs) adopted by 50 importing countries on exports of the cottonseed commodities for the year 2005 to 2014. In this study, we estimate the augmented gravity model using the ordinary least squares (OLS) and Poisson regression estimators. The results show that maximum residue limits (MRLs) have a trade increasing effect on exports of the cottonseed commodities.

scholarly journals Determination of the bifenazate insecticide in apples and cucumbers by high performance liquid chromatography

2019 ◽  
Vol 55 (4) ◽  
pp. 422-428
Author(s):  
M. F. Zayats ◽  
S. M. Leschev
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Diode Array ◽  
The European Union ◽  
Optimal Conditions ◽  
Plant Materials ◽  
Ultraviolet Detection ◽  
Maximum Residue Level ◽  
Distribution Constants

Based on the distribution constants of biphenazate, obtained experimentally and also calculated from literature data on the solubility of biphenazate in water and organic solvents, as well as experimental data on the extraction of biphenazate from plant matrices by various extractants, we selected the optimal conditions for extracting biphenazate from apples and cucumbers. The conditions for the purification of the extracts were also selected. Acetonitrile in the presence of ammonium sulfate and hexane was used for extraction of the pesticide. Purification of extracts of plant materials was carried out by partitioning between hexane and water-acetonitrile mixture. The samples obtained after this treatment were pure enough to determine the residual amounts of biphenazate in them at the maximum residue level determined in Belarus and the countries of the European Union, or lower using widespread liquid chromatography with diode-array (ultraviolet) detection.

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