摘要
目的:建立一种快速、简便的基质固相分散萃取技术-高效液相色谱法测定牛奶中8种磺胺类药物残留量的方法。包括磺胺(SA)、磺胺嘧啶(SDZ)、磺胺甲嘧啶(SMR)、磺胺二甲嘧啶(SMD)、磺胺氯哒嗪(SCP)、磺胺甲噁唑(SMZ)、磺胺二甲异噁唑(SIZ)、磺胺喹噁啉(SQX)。方法:采用新的样品前处理方法-基质固相分散萃取技术对牛奶中残留的磺胺类药物进行提取和净化,HPLC法测定。牛奶样品直接与硅酸镁吸附剂置于研钵中,经玻璃棒研磨、混匀制成半固态混合物,然后转移至垫有一层定量滤纸的玻璃注射器中,轻轻压实至一定体积,盖上一层滤纸,用正己烷洗脱除脂,真空抽滤至干,用二氯甲烷+乙酸乙酯(1+2)混合溶剂洗脱,洗脱液于全自动浓缩仪60℃挥干溶剂,用1.0 ml流动相溶解残渣,经0.45μm滤膜过滤,供HPLC分析。结果:8种磺胺类药物的回收率在68.3%～101.2%之间,相对标准偏差在2.4%～7.6%之间。线性范围除磺胺喹噁啉在0.1～10.0 mg/L之间外,其余7种均在0.05～10.0 mg/L范围内,相关系数0.9991～0.9997。结论:方法样品前处理简单、快速,定性、定量准确,分析成本低,易于推广应用。
Objective： A fast and simple determination method - matrix solid phase dispersion for extracting and cleaning, high performance liquid chromatography simultaneously analysis eight kinds of sulfonamides drug residues in milk was studied. They included sulfanilamide （SA） , sulfadiazine （SDZ） , sulfamerazine （SMR） , suffamdimidine （SMD） , sulfachlorpyridazine （SCP） , sulfamethoxazole （SMZ） , Sulfisoxazole （SIZ） , sulfaquinoxaline （ SQX ）. Methods： Milk sample was manually blended together with 2. 0 g magnesium silicate in a glass mortar using a glass pestle, a semi - solid material was obtained, the semi - solid material was packed as an SPE cartridge into a glass syringe with a piece of paper frit at the bottom, compressed it to 4 - 5 ml, covered with another piece of paper frit on the top of the mixture to produce a sample/column material, using 5 ml hexane to washing out fat in milk, the analyst were eluted with 8 ml Methylene chloride ＋ ethyl acetate （ 1 ＋ 2）, collected the eluting solvent. Vaporize to dry at 60℃ by Automated Dry Vap Concentrator System and dissolved the residues with l. 0 ml mobile phase, analysed by HPLC. Results：The recovery range of 8 SAs were 68.3%- 101.2%, while relative standard deviation were 2.4% -7. 6%. The linear range of sulfaquinoxaline was between 0. 5 mg/L to 10. 0 mg/L, the others were between 0. 05 mg/L to 10.0mg/ L. Conclusion：This method is simple, quick and accurate.
出处
《中国卫生检验杂志》
CAS
2009年第1期86-89,共4页
Chinese Journal of Health Laboratory Technology
基金
成都市卫生局重大医学联合攻关项目子课题(20080808)
成都市疾病预防控制中心重点科研项目资助(080102)
