摘要
目的：建立采用固相萃取-高效液相色谱荧光法同时测定蜂蜜中5种磺胺类药物残留的方法。方法：蜂蜜样品经醋酸-醋酸钠缓冲溶液溶解后，用C18固相萃取小柱富集、净化，用乙腈洗脱，5种磺胺类药物经荧光胺衍生后，以2％醋酸（v／v）溶液-乙腈（50／50，v／v）为流动相，在C18色谱柱上（250mm×4．6mm，5μm）分离，荧光法在λEx=405nm，λEm=495nm处测定。结果：5种磺胺类药物在0．01～0．20mg／L具有良好的线性，其相关系数均大于0．9995，加标回收率在82．0％～102．5％，RSD均小于5．3％，定量检出限为0．004mg／kg。结论：该方法具有快速、灵敏、简便、准确等优点，能满足实际工作的需要。
Objective：To establish an analytical method by high -performance liquid chromatography （HPLC） with fluorescence detection and solid - phase extraction （SPE） for the simultaneous determination of five sulfanilamide residues in honey. Methods ：The honey sample was dissolved in acetic acid/sodium acetate buffer solution, and the solution was directly loaded on SPE C18 cartridge and eluted by acetonitrile. After derivatization by fluorescamine, the five sulfanilamide derivatizations were separated on gemini C18 column （250 mm ×4. 6 mm, 5 μm） at a constant temperature of 30℃ by using a mobile phase of acetonitrile/0.2% CH3COOH （50/50, v/v） at a flow rate of 1.2 ml/min. Detection was performed on a fluorescence detector at λEx = 405 nm, λEm = 495 nm. Results：Calibration curves were linear in the range of 0.01 - 0. 20 mg/L with a correlation coefficient of more than 0. 9995 and the limits of quantification were found to be 0. 004 mg/kg for the five analytes. The extraction recoveries were between 82. 0% ~ 102. 5% and the RSD less than 5.3%. Conclusion：This method is simple, sensitive and accurate for the determination of sulfanilamide residues in honey and it can be satisfactorily applied to the routine analysis.
出处
《中国卫生检验杂志》
CAS
2007年第3期468-469,500,共3页
Chinese Journal of Health Laboratory Technology
