Yang Yi, Zhang Jing, Li Yongxin, Yin Shuo, Jiang Yang, Sun Chengjun
School of Public Health, Southwest Medical University, Luzhou 646000, China.
Anal Methods. 2021 Apr 7;13(13):1618-1624. doi: 10.1039/d1ay00154j. Epub 2021 Mar 18.
A dissolvable layered double hydroxide-based solid-phase extraction combined with high-performance liquid chromatography was developed for the analysis of minocycline, oxytetracycline, tetracycline, demeclocycline, metacycline, chlortetracycline and doxycycline in milk samples. In situ formation of the layered double hydroxide was achieved by the addition of MgCl-AlCl solution to alkaline deproteinized milk. The analytes were efficiently extracted by the Mg/Al layered double hydroxide. After centrifugation, the co-precipitates were dissolved in 0.1 mol L NaEDTA-McIlvaine buffer prior to HPLC analysis. Under optimized conditions, the method achieved low detection limits of 0.414-0.986 μg L and quantification limits of 1.38-3.29 μg L, and good recoveries of 93.5-100% with intra- and inter-day RSDs of 0.498-4.08% and 1.23-10.0%, respectively. This method is convenient, accurate, sensitive, rapid, cost-effective, eco-friendly, and suitable for the determination of seven tetracycline antibiotics in milk samples.
建立了一种基于可溶解层状双氢氧化物的固相萃取结合高效液相色谱法，用于分析牛奶样品中的米诺环素、土霉素、四环素、地美环素、美他环素、金霉素和多西环素。通过向碱性脱蛋白牛奶中加入MgCl-AlCl溶液实现层状双氢氧化物的原位形成。分析物被Mg/Al层状双氢氧化物有效萃取。离心后，共沉淀物在进行高效液相色谱分析前溶解于0.1 mol/L NaEDTA-麦氏缓冲液中。在优化条件下，该方法的检测限低至0.414 - 0.986 μg/L，定量限为1.38 - 3.29 μg/L，回收率良好，为93.5% - 100%，日内和日间相对标准偏差分别为0.498% - 4.08%和1.23% - 10.0%。该方法方便、准确、灵敏、快速、经济高效、环保，适用于牛奶样品中七种四环素类抗生素的测定。
