Abstract A rapid ultra-performance liquid chromatography (UPLC) method with simplified sample preparation procedures was developed for detection of furosine in milk. In tuning the sample preparation, nitrogen purging was not required for acid hydrolysis and the duration of acid hydrolysis was shortened. Purification by solid-phase extraction was also found to be unnecessary. UPLC parameters were optimized. The retention time of furosine was 1.866 min, with good separation from impurities in milk. The method was validated and shown to have good sensitivity, accuracy, precision, repeatability, and reproducibility. The limit of detection was 0.01 mg/L and the limit of quantification was 0.025 mg/L. The range of linearity was 0.5–5.0 mg/L (R2 = 0.9998). Milk samples spiked with different furosine levels showed recoveries of 83.96 %–93.51 %, with an overall mean recovery of 89.68 ± 0.06 %. The coefficients of variation for intraday, inter-day, and inter-laboratory determinations were 0.2 %–1.6 %, 0.5 %, and 4.0 %–8.1 %, respectively. The proposed method was utilized to quantify furosine in pasteurized, extended shelf life, and ultra-high-temperature-treated milk samples, which demonstrated that this novel UPLC method is effective for rapid determination of furosine in milk samples.

中文翻译：

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采用优化样品制备程序的快速 UPLC 方法测定牛奶中的呋喃

摘要 开发了一种简化样品制备程序的快速超高效液相色谱 (UPLC) 方法，用于检测牛奶中的呋喃氨酸。在调整样品制备时，酸水解不需要氮气吹扫，酸水解的持续时间缩短了。还发现不需要通过固相萃取进行纯化。UPLC 参数进行了优化。糠氨酸的保留时间为1.866 min，与牛奶中的杂质分离良好。该方法经过验证并显示具有良好的灵敏度、准确度、精密度、重复性和再现性。检测限为0.01 mg/L，定量限为0.025 mg/L。线性范围为 0.5–5.0 mg/L (R2 = 0.9998)。添加不同浓度呋喃的牛奶样品显示回收率为 83.96 %–93.51 %，总体平均回收率为 89.68 ± 0.06 %。日内、日间和实验室间测定的变异系数分别为 0.2%–1.6%、0.5% 和 4.0%–8.1%。所提出的方法用于定量巴氏杀菌、延长保质期和超高温处理的牛奶样品中的呋喃氨酸，这表明这种新型 UPLC 方法可有效快速测定牛奶样品中的呋喃氨酸。