固相萃取/高效液相色谱法同时测定保健食品中7种磺酰脲类降血糖药物  

Simultaneous Determination of Seven Sulfonylurea Hypoglycemic Agents in Health Care Products by Solid Phase Extraction / High Performance Liquid Chromatography

作　　者：周春燕[1] 唐柏彬[2] 郗存显[2] 陈冬东[3] 张雷[2] 彭涛[3] 王国民[2] 陈志琼[1] 

机构地区：[1]重庆医科大学药学院,重庆400016 [2]重庆出入境检验检疫局重庆市进出口食品安全工程技术研究中心,重庆400020 [3]中国检验检疫科学研究院,北京100123

出　　处：《分析测试学报》2013年第10期1212-1216,共5页Journal of Instrumental Analysis

基　　金：国家科技部科技资助项目(2012BAD33B02);质检公益性行业科研专项(201010073);重庆市科委项目(CSTC2009CB1012)

摘　　要：建立了同时测定保健食品中7种磺酰脲类降血糖药物（格列吡嗪、甲苯磺丁脲、妥拉磺脲、格列齐特、格列本脲、格列美脲和格列喹酮）的固相萃取/高效液相色谱（SPE/HPLC）分析方法.样品经甲醇超声提取,用C18固相萃取柱净化后进行HPLC分析.采用Agilent Zorbax SB-C18色谱柱（250 mm×4.6 mm,5μm）,以乙腈（A）-0.02％磷酸溶液（B）为流动相,梯度洗脱,流速1.0 mL/min,柱温30℃,检测波长228 nm.结果表明,7种目标物在0.2～20 μg/mL范围内线性关系良好,相关系数（r）大于0.999 9,检出限（LOD,S/N≥3）均为0.1 mg/kg,在5种不同基质中的加标回收率为81％～115％,相对标准偏差（RSD）小于9％.A method was established for the simultaneous determination of seven sulfonylurea hypoglycemic agents （e.g.glipizide,tolbutamide,tolazamide,gliclazide,glibenclamide,glimepiride and glurenor） in health care products by solid phase extraction/high performance liquid chromatography（SPE/HPLC）.Various samples were extracted with methanol by ultrasound,the extract was cleaned up and concentrated on an LC-C18 SPE column.The chromatographic separation was performed on an Agilent Zorbax SB-C18 column（250 mm ×4.6 mm,5 μm） using acetonitrile（A）-0.02％ phosphoric acid solution （B） as mobile phase by gradient elution at a flow rate of 1.0 mL/min,a column temperature of 30 ℃ and an ultraviolet （UV） detection wavelength of 228 nm.The seven sulfonylurea hypoglycemic agents showed good linear relationships in the range of 0.2-20 μg/mL with correlation coefficients larger than 0.999 9.The limits of detection（S/N≥3） were 0.1 mg/kg for seven target compounds.The spiked recoveries of seven target compounds in five different health care products ranged from 81％ to 115％ with relative standard deviations less than 9％.

关 键 词：固相萃取 高效液相色谱法 保健食品 磺酰脲类降血糖药物 

分 类 号：O657.72[理学—分析化学] TQ460.72[理学—化学]