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中国科技核心期刊
ISSN 1671-5187
CN 31-1881/S
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Determination of 17 Mycotoxins in Milk and Dairy Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry
LIU Ling, YE Pei, ZHANG Qiaoyan, SHEN Ying, DONG Yuying, JIANG Mengyuan, LI Wenting
Journal of Dairy Science and Technology 2023, 46 (
5
): 22-27. DOI:
10.7506/rykxyjs1671-5187-20231011-050
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27
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To establish a method for simultaneous detection of 17 mycotoxins in milk and dairy products based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Samples (5.000 0 g) were added to 20 μL of a mixed solution of isotope-labeled internal standards, extracted with 20 mL of acetonitrile-water-formic acid solution (70:29:1, V/V) by vortex shaking, salted out with 0.3 g of sodium chloride, and then centrifuged at high speed. The supernatant was passed through a 0.22 μm membrane filter, detected by triple quadrupole mass spectrometry in the multi-reaction detection mode and quantified by an internal standard method. Results: Under the optimized instrumental conditions, good linearity was observed for the 17 mycotoxins in the tested concentration ranges, with correlation coefficient (r) greater than 0.99. The limit of detection (LOD) was 0.05-6.20 μg/kg, and the limit of quantitation (LOQ) was 0.2-20.0 μg/kg. Good average recoveries (78.9%-119.5%) and precision (relative standard deviations (RSDs) 0.2%–8.4%) were achieved at three spiked levels. The method is convenient, stable, reliable and sensitive, can meet the requirements of qualitative and quantitative analysis of the 17 mycotoxins in milk and dairy products, and is suitable for laboratory monitoring of the contamination of these mycotoxins in milk and dairy products.
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Analysis of the Pollution Status of Eight Harmful Elements in Commercial Milk Fan and Milk Cake
CHEN Junxiu, LI Jie, LIU Ling, RAN Yali, LI Yi, LI Wenting
Journal of Dairy Science and Technology 2022, 45 (
3
): 19-23. DOI:
10.7506/rykxyjs1671-5187-20220427-024
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To investigate the pollution status of eight harmful elements in milk fan and milk cakes. Milk fan and milk cake were sampled from representative farmers’ markets and supermarkets in some districts or counties of a certain city. The samples were digested by a wet digestion method using graphite, and eight harmful elements including arsenic, lead, mercury, cadmium, chromium, boron, aluminum and barium in the digested samples were simultaneously detected by inductively coupled plasma mass spectrometry (ICP-MS) and quantified by an internal standard method. Neither milk fan nor milk cake samples were found to be contaminated by mercury or cadmium, and the contamination levels of boron, arsenic, barium and lead was relatively low; however, the milk fan samples were seriously polluted by aluminum and chromium, and the contamination level of barium in milk cakes was relatively high. Both milk fan and milk cake samples contained chromium, barium and lead, and the contamination level of the former was higher than that of the latter. Accordingly, relevant departments should strengthen supervision over milk fan and milk cake workshops, standardize the production processes, strictly control the potential pollution links, and strengthen supervision over pollution in the production process to ensure product quality and safety.
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