基质固相分散-高效液相色谱法测定蜂蜜中10种磺胺类药物
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余辉菊 女 副主任技师 研究方向为卫生理化检验及研究 E-mail:yucdc@163.com

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O657.7

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成都市卫生局重大医学联合攻关项目(080808);成都市疾病预防控制中心重点科研项目(080102)


Determination of ten sulfonamide residues in honey with matrix solid phase dispersion-high performance liquid chromatography
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    摘要:

    目的 建立基质固相分散-高效液相色谱法测定蜂蜜中10种磺胺类药物残留量的方法,包括磺胺、磺胺嘧啶、磺胺吡啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲氧嘧啶、磺胺间甲氧嘧啶、磺胺氯哒嗪、磺胺甲噁唑和磺胺二甲异噁唑。方法 蜂蜜样品与C18固相吸附剂于玻璃研钵中研磨均匀,得半干状混合物,装入空的固相萃取管中,盖上一层滤纸,以1+3二氯甲烷-乙酸乙酯(V/V)为洗脱剂洗脱,洗脱液经氮气吹干,用流动相溶解残渣,经0.45μm滤膜过滤,Agilent TC-C18 (4.6mm×250mm,5μm)色谱柱分离,高效液相色谱法测定。结果 10种磺胺类药物的线性范围为0.10~10mg/L,相关系数r>0.999,样品加标回收率60.0%~109.3%,相对标准偏差小于10%,方法检出限0.016~0.025mg/L,样品中磺胺类检出限为0.050~0.079mg/kg。

    Abstract:

    Objective To establish a method for the determination of 10 sulfonamides in honey, including sulfanilamide, sulfadiazine, sulfapyridine, sulfamerazine, sulfamethazine, sulfameter, sulfamonomethoxine, sulfachloropyridazine, sulfamethoxazole and sulfisoxazole, with matrix solid phase dispersion and high performance liquid chromatography. Methods Honey sample was grinded and well-distributed with a solid-phase sorbent C18 in a glass mortar to form a semi-solid mixture. The mixture was packed as a solid phase extraction (SPE) cartridge, covered with a piece of paper on the top of the mixture to produce a sample/column material; and then eluted with 20ml 1+3 methylene-ethyl acetate (V/V). The eluted materials were collected and evaporated to dry at 40℃ by nitrogen gas. The residues were dissolved in 0.5ml of mobile phase solvent and passed through a 0.45μm filter membrane, and then were separated by an Agilent TC-C18 column (4.6mm×250mm,5μm) and determined by HPLC. Results The linear ranges of 10 sulfonamides were 0.10-10.0 mg/L, r>0.999. The recovery ranges were 60.0%-109.3% and RSD<10%. The detection limits were 0.016-0.025mg/L and the quantification limits were 0.050~0.079mg/kg.

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余辉菊,杨晓松,杨胜利.基质固相分散-高效液相色谱法测定蜂蜜中10种磺胺类药物[J].中国食品卫生杂志,2011,23(2):147-150.

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  • 收稿日期:2010-08-03
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