PDF《炮制对小茴香中黄酮成分的影响 *》

提取溶剂的用量基本不影响小茴香中指标 成分的提取效率, 故最终选择

25 mL.因此, 确定 供试品最优制备方法, 如 2.3 项下供试品制备方法 所述. 3.1.2 小茴香方法学验证研究 按 2.1 项下色谱 条件测定 2.2 项下系列混合对照品溶液, 平行进样

2 次, 以对照品浓度为横坐标 X (μg/mL) , 以对照品 峰面积为纵坐标 Y, 绘制标准曲线;

小茴香中 SG、 QG 在相应浓度范围内线性关系良好 (r>

0.999) , 检 测限 (S/N=3) 分别为 0.002

7、 0.003

4 μg/mL;

定量限 (S/N=10) 分别为 0.008

1、 0.010

1 μg/mL;

方法学验 证结果均符合含量测定要求, 结果如表

1 所示. 结果表明, SG、 QG 的日内精密度(相对标准偏 差, RSD) 分别为 0.35%、 0.23%, 日间精密度 RSD 分 别为 1.34%、 0.41%;

小茴香供试品溶液在

10 ℃条件 下放置

12 h 内稳定性良好, RSD 分别为 0.45%、 0.71%;

加样回收率分别为 98.65 %、 98.31%, RSD 分 别为 1.42%、 2.26%;

该方法准确可行. 3.2 盐小茴香炮制工艺研究 系统考察了炮制过 程中的盐水比例、 炮制温度、 炮制时间对小茴香 中SG、 QG 含量的影响.采用 2.1 项下色谱条件测 定供试品溶液中两种指标成分的含量,结果如图

1 所示. 结果表明,盐水比例对盐小茴香中 SG、 QG 的 含量基本没有影响;

随着炮制温度的升高和炮制时 间的延长黄酮类成分的含量逐渐下降, 盐小茴香表 面呈焦黑色.因此, 结合生产的实际需要, 最终确定 盐小茴香的炮制工艺: 取生小茴香至炒药锅 (180~

200 ℃) 中, 均匀翻炒, 炒至微显火色, 喷淋 25%盐水

613 天津中医药Tianjin Journal of Traditional Chinese Medicine

2019 年6 月第36 卷第6 期Jun. 2019熏Vol.36 No.6 Effect of processing on Flavonoids in Fennel LI Min,DOU Zhiying,CHAI Xin,WANG Yuefei,YANG Jing (Tianjin University of Traditional Chinese Medicine,Institute of Traditional Chinese Medicine,Tianjin State Key Laboratory of Modern Chinese Medicine,Tianjin 301617,China) Abstract: [Objective] To establish a method for determining the contents of syringin and quercetin鄄3鄄O鄄glucuronide in Fennel and optimizing the processing technology of salt Fennel. [Methods] On the basis of the methodological validation of quantification of syringin and quercetin鄄3鄄O鄄glucuronide,the systematical study was performed to screen the ratio of salt and water,frying temperature and parching time. Also,the analysis of the index components was conducted in Fennel collected from the market. [Results] The optimal condition of salt鄄processing for Fennel was screened as 1∶4 for the salt water ratio,180~200 ℃ for stir鄄frying temperature and 15~20 min for parching time. Under this condition,the color of salt Fennel was deepened,occasionally scorched,slightly bulged. The contents of index components in Fennel slightly decreased by salt鄄processing. The great difference was detected of the contents of index components in Fennel from the market. [Conclusion] This study illuminated the variation of the contents of index components in the processing and the quality differences of Fennel on the market,which provided the experimental basis of the quality control and processing for the Fennel. Key words:Fennel;

salt Fennel;

syringin;

quercetin鄄3鄄O鄄glucuronide 表1SG、QG 的线性回归方程、线性范围、相关系数、检测限、定量限、精密度、稳定性、加样回收率结果 Tab.1 Linearity,LOD and LOQ,intra- and inter-day precision,stability,recovery of SG and QG 化合物 标准曲线 线性范围 (μg/mL) 相关系数 (r) 检测限 LOD (μg/mL) 定量限 LOQ (μg/mL) 精密度 (RSD, %) 稳定性 (RSD, %) 平均加样回收率 (%, n=6) 日内 (n=6) 日间 (n=3) SG =13 234X-269.07 1.551~99.30 0.999 0.002