高效液相色谱-二极管阵列法测定保健酒中的舒林酸  

Determination of Sulindac in Health Liquor Using HPLC-PAD

作　　者：郭杰标[1] 蓝献泉 刘旺培 严晓明 何颖娟[1] 

机构地区：[1]韶关学院,广东韶关512005 [2]韶关市食品药品检验所,广东韶关512026

出　　处：《安徽农业科学》2014年第22期7550-7552,共3页Journal of Anhui Agricultural Sciences

基　　金：广东省自然科学基金项目(S2011040001362);韶关市科技计划项目(2013CX/K97)

摘　　要：[目的]建立保健食品中违禁添加舒林酸的液相检测方法.[方法]通过酸性条件氯仿和碱性水溶液两步液-液萃取,从保健酒中提取和净化舒林酸.使用Kromasil 100-5C18（250×4.6 mm E74572）色谱柱,流动相为0.06 mol/L醋酸缓冲液（pH 4.0）-甲醇-乙腈（59∶ 29∶12,V/V/V）;流速为0.8 ml/ min进行分离;检测波长为328 nm.根据色谱峰保留值比对和加标试验,结合二极管阵列扫描图谱对可疑样品定性,并根据外标法峰面积定量检测.[结果]检品和基质成分实现了基线分离,最低检测限为0.5 μg/ml,工作曲线的线性范围：10～160 μg/ml（R2=0.9996）,回收率88.6％～91.6％.[结论]该研究建立的方法准确、可靠,适用于检测保健品中违法添加的舒林酸.[Objective] To develop a liquid chromatographic method coupled with photodiode array detector for identification of illegal adulterated sulindac in healthy food.[Method] Two-step liquid-liquid extractions were employed to purify sulindac from samples using chloroform （in acidic condition） following aqueous solution （in alkaline condition）,respectively.Chromatographic separation was achieved on a Kromasil 100-5C18 column（250 × 4.6 mm E74572） with the mobile phase of acetonitrile-methanol-0.06 mol/L acetate buffer （pH 4.0） （12/29/59,V/V/V）,at a flow rate of 0.8 ml/min.The eluant was detected at 328 nm.Retention time and standard addition result combined with PAD-scanning graph were applied to verify sulindac.Quantitation of sulindac was attempted by external standard method.[Result] The results showed as follows：the limit of quantitation was 0.5 ng/ml.The recovery of sulindac from health liquor was ranging from 88.6％ to 91.6％.[Conclusion] The method is suitable in determination of sulindac as adulterants in health liquor due to its accuracy and reliability.

关 键 词：功能食品 舒林酸 违法添加 液-液萃取 色谱检测 

分 类 号：S609.9[农业科学—园艺学] R155.15[医药卫生—营养与食品卫生学]