Rapid trace level determination of sulfonamide residues in honey with online extraction using short C-18 column by high-performance liquid chromatography with fluorescence detection.
Rapid trace level determination of sulfonamide residues in honey with online extraction using short C-18 column by high-performance liquid chromatography with fluorescence detection.
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DOI：
10.1016/j.chroma.2013.09.020
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发表时间：
2013-11
期刊：
影响因子：
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通讯作者：
M. Sajid;Na Na-Na;M. Safdar;Xin Lu;Lin Ma;Lan He;J. Ouyang
中科院分区：
文献类型：
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作者：
M. Sajid;Na Na-Na;M. Safdar;Xin Lu;Lin Ma;Lan He;J. Ouyang
建立了一种灵敏、廉价的蜂蜜中磺胺残留量的在线提取-高效液相色谱-荧光检测方法。在样品制备过程中，用酸水解法打破了蜂蜜糖与磺胺类药物之间的N-糖苷键，并在蜂蜜基质中用柠檬酸缓冲液(0.5M)在pH值为3.5的条件下进行了磺胺类药物的衍生化反应。色谱柱为Zorbax Extended C-18(250 mm×34.6 mm；5μm)，流动相为乙腈-醋酸盐缓冲液(pH 4.50，20 mm)。采用Zorbax Extended C-18(12 mm×34.6 mm；5μm)色谱柱，利用二位阀在线提取蜂蜜中15种磺胺类药物残留。蜂蜜中磺胺残留量的最低定量限小于3 ng g−1，加标回收率为磺胺的80%~磺胺氯吡嗪的100%。该方法对所研究的磺胺类药物具有良好的线性关系，相关系数为0.993。
A sensitive and inexpensive quantification method with online extraction using a short C-18 column for sulfonamide residues in honey by high performance liquid chromatography with fluorescence detector was developed and validated. In sample preparation, acid hydrolysis was used to break the N-glycoside bond between the honey sugar and sulfonamide drugs and derivatization of sulfonamide residues with fluorescamine was conducted at pH 3.5 using a citrate buffer (0.5 M) in the honey matrix. The chromatography was carried out on Zorbax Extended C-18 (250 mm × 4.6 mm; 5 μm) column, using a mixture of acetonitrile and an acetate buffer (pH 4.50, 20 mM) as a mobile phase. A Zorbax Extended C-18 (12 mm × 4.6 mm; 5 μm) column was used for online extraction of fifteen sulfonamide residues from honey sample with the help of a two position valve. The limit of quantification of sulfonamide residues in honey was less than 3 ng g−1, and the percentage recovery of study compounds in spiked honey sample was from 80% for sulfacetamide to 100% of sulfachloropyridazine. The developed method has excellent linearity for all studied sulfonamides with a correlation coefficient 0.993.