The Health Bureau of Kaohsiung County Government, No. 834-1, Chengcing Road, Niaosong, Kaohsiung County 833, Taiwan.
J Chromatogr A. 2010 Dec 3;1217(49):7812-5. doi: 10.1016/j.chroma.2010.10.008. Epub 2010 Oct 31.
A simple sugaring-out assisted liquid-liquid extraction method combined with high-performance liquid-chromatography with fluorescence detection (HPLC-FL) was developed for the extraction and determination of sulfonamides in honey. Sample preparation consisted of acid hydrolysis to release sugar-bound sulfonamides. After derivatization with fluorescamine, the derivatives were partitioned into the organic layer under the honey (sugar)/water/acetonitrile system. The clear organic extract obtained by centrifugation could be injected into the HPLC system either directly or after dilution. Linearity was obtained with the coefficient of determination (R(2)) higher than 0.998 from 2 to 200 ng/mL. Under the optimal conditions, recoveries were determined for honey fortified at three levels (5, 20, and 100 ng/g) were 80.9-99.6% with coefficients of variation of 0.3-4.4%. Limits of detection for the sulfonamides studied were found to range from 0.6 to 0.9 ng/g.
建立了一种简单的加糖辅助液-液萃取方法，结合高效液相色谱荧光检测（HPLC-FL），用于从蜂蜜中提取和测定磺胺类药物。样品制备包括酸水解以释放与糖结合的磺胺类药物。用荧光胺衍生化后，衍生物在蜂蜜（糖）/水/乙腈体系下分配到有机层中。通过离心获得的澄清有机提取物可以直接或稀释后注入 HPLC 系统。在 2 至 200ng/mL 范围内，线性相关系数（R²）高于 0.998。在最佳条件下，在三个水平（5、20 和 100ng/g）下对蜂蜜进行加标，回收率为 80.9-99.6%，变异系数为 0.3-4.4%。研究的磺胺类药物的检测限范围为 0.6 至 0.9ng/g。
