基于限进介质-磁性微球的磁分散萃取-液相色谱法同时检测牛奶中四环素类药物残留

Simultaneous determination of tetracyclines residues in milk using magnetic dispersion extraction – liquid chromatography based on restricted access media-magnetic microsphere access media-magnetic microsphere

中文关键词:  四环素类抗生素  磁分散萃取  限进材料  磁性微球  高效液相色谱法  牛奶

英文关键词:tetracyclines  magnetic dispersion extraction  restricted access materials  magnetic microsphere  high performance liquid chromatography  milk

中文摘要:

      目的 建立了一种集净化和富集为一体的限进介质磁性微球(RAM-MMs)制备方法和磁分散萃取牛奶中四环素类抗生素方法。方法 采用悬浮聚合法, 制备了表面亲水的磁性高分子微球。以牛奶为原料, 样品经三氯乙酸和Na2EDTA - McIlvaine缓冲溶液提取, 磁性微球净化富集后, 用C18色谱柱分离, 以甲醇: 乙腈: 10 mmol/L草酸(5:25:70, v:v:v)为流动相进行检测, 外标法定量。结果 在最佳条件下, 获得了较好的净化效果和较高的富集因子(13.2)。在0.1、0.2、0.5 mg/kg三个加标水平下, 此方法回收率为76.4%~95.84%, 相对标准偏差为2.72%~6.81%, 方法检出限(S/N=3)和定量限(S/N=10)分别为5.71~11.18 mg/kg和19.02~37.28 mg/kg。结论 该方法简便快速、灵敏可靠、经济有效, 适用于原奶中四环素类抗生素残留的测定。

英文摘要:

      Objective A novel synthesis method of restricted access media-magnetic microspheres (RAM-MMs) with enrichment and clean-up effect was developed for magnetic dispersion extraction (MDE) of tetracyclines residues in milk. Methods The surface hydrophilic magnetic polymer microspheres were prepared by suspension polymerization. Tetracyclines were extracted from milk samples with trichloroacetic acid and Na2EDTA-McIlvaine buffer solution, and then detected by HPLC-UV with external standard method using me-thanol:acetonitrile:10 mmol/L oxalic acid solution (5:25:70, v:v:v) as mobile phase after being cleaned up with RAM-MMs. Results An enrichment factor of 13.2 along with a good sample clean-up was obtained under the optimized conditions. The average recoveries of three tetracyclines antibiotics spiked milk at 0.1, 0.2 mg/kg and 0.5 mg/kg were in the range of 76.4%?95.84% with the precision of 2.72%?6.81%. The limits of detection (S/N=3) and quantitation (S/N=10) of the proposed method were in a range of 5.71?11.18 μg/kg and 19.02?37.28 μg/kg,