固相萃取-高效液相色谱法同时测定降糖茶中7种胰岛素分泌促进剂  

Simultaneous Determination of 7 Insulinotropic Agents in Jiangtang Tea by Solid Phase Extraction-High Performance Liquid Chromatography

作　　者：周春燕[1] 郗存显[2] 唐柏彬[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：《分析化学》2013年第11期1704-1708,共5页Chinese Journal of Analytical Chemistry

基　　金：国家科技部<功能食品有效成份检测和鉴伪技术研究>(No.2012BAD33B02);质检公益性行业科研专项(No.201010073);重庆市科委(No.CSTC2009CB1012)资助项目

摘　　要：建立了固相萃取-高效液相色谱（SPE-HPLC）同时测定降糖茶中7种胰岛素分泌促进剂的方法.试样经甲醇超声提取、NH2固相萃取柱净化后,采用Agilent ZorbaxSB-C18色谱柱（250 mn×4.6 mm,5μm）进行分离,以乙腈-0.02％磷酸溶液为流动相,梯度洗脱,流速1.0 mL/min,柱温30℃,检测波长228 nm.结果表明：在0.2～20.0 mg/L范围内,7种组分的线性相关系数均大于0.9999;检出限为0.10 ～0.13 mg/kg;定量限为0.30 ～0.40 mg/kg.添加浓度水平为1.0,2.0,5.0 mg/kg时,回收率为84.5％ ～ 110.0％;RSD＜5.0％.A solid phase extraction coupled with high performance liquid chromatographic method has been developed for the simultaneous determination of 7 insulinotropie agents in Jiangtang Tea. As a result, various samples were extracted with methanol by ultrasound, and the extract was cleaned up on an NH2 SPE column. The chromatographic separation was performed on an Agilent Zorbax SB-C18 column （250 mm×4.6 mm, 5 μm） using aeetonitrile-0.02% phosphoric acid solution with gradient elution as the mobile phase with a flow rate at 1.0 mL/min, column temperature at 30℃and ultraviolet （UV） detection at wavelength of 228 nm. There were good linear correlations between the concentrations and peak areas of the seven insulinotropie agents, the linear range was 0.2-20.0 mg/L and correlation coefficients were above 0. 9999. The limits of detection （LOD） of the seven insulinotropic agents were in the range of 0. 10-0. 13 mg/kg, limits of quantification （LOQ） were in the range of 0.30-0.40 mg/kg. The average recoveries for all components were 84.5%-110.0% and the relative standard deviations （RSDs） were less than 5.0% at spiked levels of 1.0, 2.0 and 5.0 mg/kg.

关 键 词：固相萃取 高效液相色谱法 降糖茶 胰岛素分泌促进剂 

分 类 号：TS272.7[农业科学—茶叶生产加工] O657.72[轻工技术与工程—农产品加工及贮藏工程]