Phiroonsoontorn Nattaphorn, Sansuk Sira, Santaladchaiyakit Yanawath, Srijaranai Supalax
Materials Chemistry Research Center, Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science, Khon Kaen University, Khon Kaen, 40002, Thailand.
Department of Chemistry, Faculty of Engineering, Rajamangala University of Technology Isan, Khon Kaen, 40000, Thailand.
J Chromatogr A. 2017 Oct 13;1519:38-44. doi: 10.1016/j.chroma.2017.09.005. Epub 2017 Sep 4.
This research presents a simple and green in situ solid phase extraction (is-SPE) combined with high-performance liquid chromatography (HPLC) for the simultaneous analysis of tetracyclines (TCs) including tetracycline, oxytetracycline, and chlortetracycline. In is-SPE, TCs were efficiently extracted through the precipitation formation of dissolvable layered double hydroxides (LDHs) by mixing the LDH components such as magnesium and aluminum ions (both in metal chloride salts) thoroughly in an alkaline sample solution. After the centrifugation, the precipitate was completely dissolved with trifluoroacetic acid to release the enriched TCs, and then analyzed by HPLC. Under optimized conditions, this method gave good enrichment factors (EFs) of 41-93 with low limits of detection (LODs) of 0.7-6μg/L and limits of quantitation (LOQs) of 3-15μg/L. Also, the proposed method was successfully applied for the determination of TCs in water and milk samples with the recoveries ranging from 81.7-108.1% for water and 55.7-88.7% for milk.
本研究提出了一种简单、绿色的原位固相萃取（is-SPE）与高效液相色谱（HPLC）联用的方法，用于同时分析四环素类药物（TCs），包括四环素、土霉素和金霉素。在原位固相萃取中，通过在碱性样品溶液中充分混合镁离子和铝离子等层状双氢氧化物（LDHs）的成分，形成可溶解的层状双氢氧化物沉淀，从而有效地萃取四环素类药物。离心后，沉淀用三氟乙酸完全溶解以释放富集的四环素类药物，然后通过高效液相色谱进行分析。在优化条件下，该方法具有41-93的良好富集因子（EFs），检测限（LODs）低至0.7-6μg/L，定量限（LOQs）为3-15μg/L。此外，该方法成功应用于水和牛奶样品中四环素类药物的测定，水样品的回收率为81.7-108.1%，牛奶样品的回收率为55.7-88.7%。
