Identification of Cationic and Anionic Surfactants by Chromatography–Mass-Spectrometry in the Microextraction–Fluorimetry Screening of Water and Food Products

2021 ◽  
Vol 76 (5) ◽  
pp. 592-602
Author(s):  
V. G. Amelin ◽  
Z. A. Ch. Shogah ◽  
D. S. Bol’shakov
2021 ◽  
Vol 65 (4) ◽  
pp. 388-393
Author(s):  
Valerii N. Rakitskii ◽  
Natalia E. Fedorova

Introduction. Analytical control of chemical contamination is essential in ensuring the safety of food products manufactured using pesticides. The development and testing of new methodological techniques for multicomponent measurement of the levels of residual amounts of biologically active ingredients are constantly in the field of view of analysts. Research objectives. To assess the suitability of the QuEChERS methodological approaches for the determination of a wide range of pesticides of various structures and physicochemical properties (up to 50 names of active substances) in food products and food raw materials of various compositions and origins (fruits, vegetables, cereals, rice, tea, coffee, milk, eggs and their derivatives, meat, offal). Material and methods. The measurements were carried out by tandem liquid chromatography-mass spectrometry and gas chromatography with a mass-selective detector, focused on screening and quantifying trace amounts of pesticides. The sample preparation procedure for analysis was carried out according to the QuEChERS method. Results. Multimethods have been created for the determination of residual amounts of pesticides in cereal grains (40 substances), fruits of vegetables and fruits (27 compounds), fruits of citrus crops (50 ingredients), 2,4-D acid in milk, eggs and by-products, fipronil and its toxic metabolite - sulfone in eggs, products of their processing (melange, dry egg white), muscle tissue and offal. The developments have supplemented the list of certified measurement methods included in the unified information fund of measurement methods of the Russian Federation. Conclusions. The unification of analytical methods for preparing samples of food products of various composition and origin for analysis, instrumentation of analytical laboratories with liquid and gas chromatography-mass spectrometry systems expand the possibilities of introducing group methods, ensure the readiness of testing centres to perform multi-purpose tests to identify and measure pesticide levels.


Foods ◽  
2018 ◽  
Vol 7 (11) ◽  
pp. 185 ◽  
Author(s):  
Najah Al-Mhanna ◽  
Holger Huebner ◽  
Rainer Buchholz

The aim of this study is to develop and optimise a method of sugar content determination in food products. Date juice (syrup) was used as a sample natural food resource for the analysis because of its potential usage as an alternative substrate for a variety of fermentation processes. Hence, qualifying and quantifying its sugar content is a crucial step. Therefore, gas chromatography mass spectrometry (GCMS) was used as a pre-qualitative method to identify the types of sugar in the date sample. The results demonstrate that the analysed date juice contains glucose, fructose and sucrose. This analysis was obtained by measuring the retention time of individual standard sugar samples such as glucose, fructose, mannose and sucrose. In addition, the mass spectra of the standard and date juice samples contained characteristic fragments of glucose, fructose and sucrose. Thus, GCMS results determined the appropriate enzymatic assays for quantifying the sugars in date juice. These results were similar to those of the two enzymatic methods (standard enzymatic assay and measuring the change in pH by CL10 analyser). Therefore, they confirmed the identified sugars and provided the sugar contents of the sample. Consequently, sugar quantification results indicate that 1 g of date juice sample contains a total of 0.5275–0.5507 g of six-carbon sugars (glucose + fructose) and 0.064–0.068 g of sucrose. As a consequence, the total sugar content in 1 g of date juice is 0.600–0.615 g. These results are comparable to the sample analysis that is provided by the date juice production company.


2010 ◽  
Vol 76 (22) ◽  
pp. 7466-7472 ◽  
Author(s):  
Elisabeth G. Biesta-Peters ◽  
Martine W. Reij ◽  
Richard H. Blaauw ◽  
Paul H. in ′t Veld ◽  
Andreja Rajkovic ◽  
...  

ABSTRACT Bacillus cereus produces the emetic toxin cereulide, a cyclic dodecadepsipeptide that can act as a K+ ionophore, dissipating the transmembrane potential in mitochondria of eukaryotic cells. Because pure cereulide has not been commercially available, cereulide content in food samples has been expressed in valinomycin equivalents, a highly similar cyclic potassium ionophore that is commercially available. This research tested the biological activity of synthetic cereulide and validated its use as a standard in the quantification of cereulide contents in food samples. The synthesis route consists of 10 steps that result in a high yield of synthetic cereulide that showed biological activity in the HEp-2 cell assay and the boar sperm motility assay. The activity is different in both methods, which may be attributed to differences in K+ content of the test media used. Using cereulide or valinomycin as a standard to quantify cereulide based on liquid chromatography-mass spectrometry (LC-MS), the concentration determined with cereulide as a standard was on average 89.9% of the concentration determined using valinomycin as a standard. The recovery experiments using cereulide-spiked food products and acetonitrile as extraction solute showed that the LC-MS method with cereulide as a standard is a reliable and accurate method to quantify cereulide in food, because the recovery rate was close to 100% over a wide concentration range.


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