High-Performance Liquid Chromatography versus Other Modern Analytical Methods for Determination of Pesticides

Author(s):  
Tomasz Tuzimski ◽  
Joseph Sherma
2020 ◽  
Vol 86 (8) ◽  
pp. 72-79
Author(s):  
M. Yu. Medvedevskikh ◽  
M. P. Krasheninina ◽  
A. S. Sergeeva ◽  
V. B. Baranovskaya

The study continues the research previously published in the article «Validation of analytical methods: the international requirements» (Zavod. Lab. Diagn. Mater. 2018. Vol. 84. No. 12, pp. 25 – 31). We consider the procedure and the results of validation of the measurement procedure for determination of the residual content of enrofloxacin in food using high performance liquid chromatography with mass spectrometric detection. The program of experimental studies and calculation formulas necessary to assess the metrological characteristics of the method are presented. Validation included assessment of the detection limit, quantitation limit, decision limit, capability of enrofloxacin detection in food samples in accordance with GOST 32797–2014 «Food products, food raw materials. Method for the determination of the residual content of quinolones using high performance liquid chromatography with a mass spectrometric detector». The linearity of the calibration characteristic within the measurement range is demonstrated using the regression analysis procedure. The values of the accuracy indicators and the measurement range specified in GOST 32797–2014 were confirmed when the method was implemented in a testing laboratory.


Author(s):  
S. Senin ◽  
V. Danchuk ◽  
S. Midyk ◽  
V. Ushkalov ◽  
O. Iakubchak

The dairy industry of Ukraine is developing dynamically, its needs for the quality of raw materials are growing significantly. Detection of mycotoxins in raw milk is one of the main indicators of its safety. The high degree of toxicity of mycotoxins is a threat to the health of the lactating animal, so a large number of them are excreted in milk. If we talk about ruminants, the vast majority of mycotoxins are utilized by microorganisms of the pancreas, which does not occur in monogastric animals, so the list of mycotoxins in their milk can be much wider than the secretion of mammalian mammals. To date, the maximum permissible levels (MRLs) of mycotoxins in raw milk and dairy products have been established. Thus, a comprehensive determination of the content of mycotoxins in the secretion of the breast has not only technological but also important diagnostic value. Milk sample preparation is the most important step in the determination of mycotoxins and consists of sampling, extraction and purification from impurities. For the extraction of aflatoxins, the method of liquid extraction with acetonitrile or chloroform is used. Purification of extracts is carried out on immunoaffinity columns, cartridges with special sorbents or using certain manufacturers (MycoSep®).Enzyme-linked immunosorbent assay and high-performance liquid chromatography with fluorescence detection are used to determine aflatoxin B1 and M1 in raw milk of cows. However, all these methods have a number of disadvantages, namely: long and expensive sample preparation and insufficiently high selectivity. Currently, the complex determination of mycotoxins in various matrices by high-performance liquid chromatography with mass spectrometric detection (LC-MS/MS) and the use of modified QuEChERS sample preparation is gaining popularity. The advantage of this technique is the combination of faster and cheaper sample preparation of QuEChERS samples with highly selective LC-MS/MS chromatography. Key words: mycotoxins, raw milk, analytical methods, QuEChERS.


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