固相萃取-高效液相色谱法同时测定减肥功能食品中五种违禁药物  

Simultaneous Determination of Five Illegal Drugs in Weight Control Foods with Solid Phase Extraction-high Performance Liquid Chromatography

作　　者：王媛[1] 张文韬[1,2] 李斯特[1] 李阳[1] 孙成均[1] 

机构地区：[1]四川大学华西公共卫生学院卫生检验学教研室,成都610041 [2]成都市龙泉驿区疾病预防控制中心

出　　处：《四川大学学报（医学版）》2010年第5期873-876,895,共5页Journal of Sichuan University(Medical Sciences)

基　　金：国家科技支撑计划课题(编号2006BAD27B02)资助

摘　　要：目的建立同时测定减肥功能食品中违禁添加药物双氢克尿噻、呋噻米、克罗帕米、布美他尼和盐酸西布曲明的固相萃取-高效液相色谱法。方法样品经2%磷酸-甲醇混合溶液(1∶1,V/V)超声提取并高速离心后,上清液经MCX固相萃取柱净化,然后经弱氮气流吹至近干,用2%磷酸-甲醇(1∶1,V/V)混合溶液定容、漩涡混匀、12 000 r/min离心后取上清液进样分析。色谱条件:分离柱为Phenomenex C18(250×4.60 mm,5μm)色谱柱;流动相为0.02 mol/L磷酸二氢钾缓冲液-乙腈,梯度洗脱;柱温40℃;流速1.0 mL/min。标准曲线法定量。结果 5种违禁添加药物在0.25~100μg/mL范围内呈良好线性关系(r≥0.999),检出限为5.2~108μg/kg,平均回收率范围为86.5%~113.1%,相对标准偏差(RSD)为1.6%~8.9%。结论本法选择性好、灵敏度高、重现性好,适用于减肥功能食品中5种违禁药物的同时检测。Objective To develop a method for simultaneous determination of hydrochlorothiazide,furosemide,clopamide,bumetanide and sibutramine hydrochloride in weight control foods with solid phase extraction high performance liquid chromatography.Methods The analytes in the samples were extracted with 2% phosphoric acid-methanol(1∶1,V/V) solution ultrasonically and centrifuged.The extracts were clean-up with Osis MCX SPE columns,concentrated under weak N2 stream,and reconstituted with 2% phosphoric acid-methanol(1∶1,V/V) solution,vortex mixing and centrifugation at 12 000 r/min.The high performance liquid chromatography was performed with Phenomenex C18(250×4.60 mm,5 μm)as separation column,0.02 mol/L acetonitrile potassium dihydrogen phosphate buffer as mobile phase,gradient elution of 1.0 mL/min for the flow rate,and 40 ℃ for the column temperature.The standard curve method was used for the quantitative analysis.Results A good linear range appeared for the five analytes from 0.25 to 100 μg/mL (r≥0.999).The detection limits were 5.2-108 μg/kg.The average recoveries were 86.5%-113.1%,with the relative standard deviations of 1.6%-8.9%.Conclusion The proposed method is a reliable method with high selectivity and high sensitivity for the detection of the five illegal chemicals in the weight control foods.

关 键 词：高效液相色谱法 固相萃取 减肥功能食品 违禁添加药物 利尿剂 

分 类 号：R155[医药卫生—营养与食品卫生学]