配制酒中非法添加淫羊藿的鉴别及含量测定

Identification and determination of epimedium illegally added in mixed liquor

中文关键词:  高效液相色谱法  配制酒  淫羊藿  鉴别

英文关键词:high performance liquid chromatograph  mixed liquor  epimedium  identification

中文摘要:

      目的 建立高效液相色谱法鉴别配制酒中非法添加淫羊藿及测定淫羊藿7种特征组分的分析方法。方法 样品经水浴蒸干后, 用甲醇溶液溶解残渣, 提取液离心, 过滤, 上机测定, Waters Symmetry Shield C18 (250 mm×4.6 mm, 5 μm)色谱柱进行分离, 甲醇和纯水为流动相梯度洗脱, 外标法定量测定。结果 7种化合物的线性检测范围最高浓度为100.00 μg/mL, 相关系数r2＞0.99, 定量限为0.05～0.08 μg/g, 于1、2、10倍定量限3个添加水平下进行加标回收实验, 7种化合物平均回收率为92.64%~107.21%, 相对标准偏差(relative standard deviation, RSD)为0.75%~2.86%。结论 该方法操作方便、简单、灵敏度高、重复性好, 满足配制酒中非法添加淫羊藿中药材的含量测定, 为配制酒的科学监管提供有效的技术支撑。

英文摘要:

      Objective To establish a method for the identification of illegally added epimedium in mixed liquor and determination of 7 characteristic components of epimedium by high performance liquid chromatography. Methods The sample was evaporated to dryness in water bath, the residue was dissolved in methanol solution, the extract was centrifuged, filtered, separated on a Waters Symmetry Shield C18 (250 mm×4.6 mm, 5 μm) column, eluted with mobile phase of methanol and water, and quantified by external standard method. Results The highest concentration in the linear detection range of 7 compounds was 100.00 μg/mL, the correlation coefficient r2>0.99, and the limits of quantification were 0.05-0.08 μg/g. The recovery tests were carried out at three levels of 1, 2 and 10 times the limit of quantification, and the average recoveries of 7 compounds were 92.64%?107.21%, with relative standard deviations (RSDs) of 0.75%?2.86%. Conclusion The method is convenient and simple to operate, with high sensitivity and good repeatability, it can meet the identification requirement of illegally added epimedium in mixed liquor, and provide effective technical support for scientific supervision of mixed liquor.