采用微波辅助 HCl 水解和超高效液相色谱法快速测定牛奶中的呋塞米。

Rapid determination of furosine in milk using microwave-assisted HCl hydrolysis and ultra-performance liquid chromatography.

机构信息

Key Laboratory of Quality and Safety Control for Milk and Dairy Products of Ministry of Agriculture and Rural Affairs, Institute of Animal Sciences, Chinese Academy of Agricultural Sciences, Beijing 100193, P. R. China; College of Animal Science, Xinjiang Agriculture University, Urumchi 830091, P. R. China; Institute of Quality Standard and Testing Technology for Agro-Products, Shandong Academy of Agricultural Sciences, Jinan 250100, P. R. China; Laboratory of Quality and Safety Risk Assessment for Dairy Products of Ministry of Agriculture and Rural Affairs, Institute of Animal Sciences, Chinese Academy of Agricultural Sciences, Beijing 100193, P. R. China.

Key Laboratory of Quality and Safety Control for Milk and Dairy Products of Ministry of Agriculture and Rural Affairs, Institute of Animal Sciences, Chinese Academy of Agricultural Sciences, Beijing 100193, P. R. China; Laboratory of Quality and Safety Risk Assessment for Dairy Products of Ministry of Agriculture and Rural Affairs, Institute of Animal Sciences, Chinese Academy of Agricultural Sciences, Beijing 100193, P. R. China.

出版信息

J Dairy Sci. 2020 Dec;103(12):11086-11093. doi: 10.3168/jds.2020-18614. Epub 2020 Oct 15.

DOI:10.3168/jds.2020-18614

PMID:33069412

Abstract

Because the conventional methods for furosine analysis are time-consuming, a modified method is presented to improve analysis efficiency. Microwave-assisted HCl hydrolysis was performed at 140, 150, and 160°C for 10 to 200 min, with 6, 8, or 9 M HCl. The hydrolysate purification process was carried out using only paper and membrane filtration. An ultra-performance liquid chromatography (UPLC) system was used to achieve rapid analysis of furosine. The results showed that microwave-assisted HCl hydrolysis at 8 M and 160°C led to a stable furosine yield and took only 40 min. The UPLC analysis was completed in 8 min. The modified method was validated and obtained limit of detection at 3 µg/L, limit of quantitation of 10 µg/L, linearity range of 0.2 to 5.0 mg/L, 80.5 to 94.2% recoveries from spiked samples, and coefficients of variation of 2.2 to 6.8%. The modified method is rapid and reliable for the determination of furosine in milk.

摘要

由于常规的呋塞米分析方法耗时较长，因此提出了一种改良方法以提高分析效率。在 140、150 和 160°C 下使用微波辅助 HCl 水解 10 至 200 分钟，使用 6、8 或 9 M HCl。水解产物的纯化过程仅使用滤纸和膜过滤进行。采用超高效液相色谱（UPLC）系统实现呋塞米的快速分析。结果表明，在 8 M 和 160°C 下进行微波辅助 HCl 水解可得到稳定的呋塞米产率，仅需 40 分钟。UPLC 分析在 8 分钟内完成。对改良方法进行了验证，检测限为 3μg/L，定量限为 10μg/L，线性范围为 0.2 至 5.0mg/L，从加标样品中回收率为 80.5%至 94.2%，变异系数为 2.2%至 6.8%。改良方法快速可靠，可用于牛奶中呋塞米的测定。