高效液相色谱-二极管阵列法测定保健酒中的舒林酸

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0.5μg/ml,工作曲线的线性范围:10~160μg/ml(R2=0.999 6),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。

Determination of Sulindac in Health Liquor Using HPLC-PAD

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.