痛痒消洗剂的制备工艺和质量标准研究*

作者：张静宜1,2,3，贾淑珍1，庄 宁4，魏艳婷5，程 杰1,2,3

单位：1.河北省中医院，河北 石家庄 050000； 2.河北省中医药管理局中药评价及转化重点研究室，河北 石家庄 050000； 3.河北省中药制剂产业技术研究院，河北 石家庄 050000； 4.河北国金药业有限责任公司，河北 邢台 054000； 5.石家庄市第四医院，河北 石家庄 050000

引用：引用：张静宜，贾淑珍，庄宁，魏艳婷，程杰.痛痒消洗剂的制备工艺和质量标准研究[J].中医药导报,2025,31(8):86-92.

DOI：10.13862/j.cn43-1446/r.2025.08.014

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摘要：

目的：建立痛痒消洗剂的制备工艺方法和质量控制标准。方法：以没食子酸、龙胆苦苷、马钱苷酸、升麻素苷、阿魏酸、5-O-甲基维斯阿米醇苷的含量及干膏得率为指标，采用Box-Behnken响应面试验，以提取时间、浸泡时间和加水量作为影响因素，通过信息熵法对其进行加权，计算综合评分，通过响应面模型分析各影响因素间的交互作用，筛选痛痒消洗剂的最佳提取工艺；采用单因素试验考察过滤与浓缩方式，确定制备工艺；采用薄层色谱（TLC）法对处方中的五倍子和苦参进行薄层定性鉴别；采用高效液相色谱（HPLC）法对有效成分没食子酸、龙胆苦苷、马钱苷酸、升麻素苷、阿魏酸、5-O-甲基维斯阿米醇苷进行含量测定。结果：最佳提取工艺参数为第一次加9倍量水，浸泡45 min，煎煮80 min，第二次加7倍量水，煎煮40 min；采用200目滤布过滤，减压（压强为0.05 mbar）浓缩温度控制在55～60 ℃。苦参、五倍子的TLC图斑点清晰且阴性无干扰。没食子酸、龙胆苦苷、马钱苷酸、升麻素苷、阿魏酸、5-O-甲基维斯阿米醇苷分别在3.76～11.28、0.70～3.48、0.61～3.06、0.02～0.08、0.07～0.36、0.07～0.35 μg/mL范围内线性关系良好（r≥0.999 5），精密度、重复性、稳定性的RSD＜2%；平均加样回收率分别为102.46%、101.40%、102.45%、102.01%、102.72%、101.56%，RSD＜3%（n=6）。结论：该制备工艺稳定、可行，且建立的定性定量方法可靠、便捷、专属性强，可作为痛痒消洗剂的质量控制方法。

关键词：痛痒消洗剂；制备工艺；质量标准；薄层色谱；高效液相色谱

Abstract：

Objective: To optimize the preparation technology and set up the quality standard of Tongyangxiao Lotion (痛痒消洗剂). Methods: Box-Behnken response surface methodology was used to design the experiment with the extraction time, soaking time, and additional amount of water as the investigation factors, and with the content of the extraction rate and dry paste rate of gallic acid, gentiopicrin, maggianin, ferulic acid, cosimin side and 5-O-methylwisamitol side as the evaluation indexes. The weight coefficient was determined by the information entropy method, and the comprehensive score was calculated. The interaction among the influencing factors was analyzed by the response surface model, the optimal extraction process was obtained. Single factor test was used to investigate the filtration and concentration, and preparation process was carried out. Kushen (Sophorae flavescentis radix) and Wubeizi (Galla chinensis) were identified by thin layer chromatography (TLC) method, and the content of active ingredient was determined by High performance liquid chromatography (HPLC) method. Results: The optimal extraction process is as follows: using 9 times the amount of water for 45 min, and extraction 80 min at the first time and 7 times the amount of water decocting 40 min for the second time; Filter with a 200 mesh filter cloth and controlling the concentration temperature in the range of 55-60 ℃ under reduced pressure (pressure of 0.05 mbar). TLC can identify these extractions, the spots of Kushen (Sophorae flavescentis radix) and Wubeizi (Galla chinensis) were clear, and their negative control showed no interference. The calibration curve of gallic acid, loganin acid, gentiopicroside, ferulic acid, coumarin glycoside, 5-O-methylvisamminol glycoside were at concentrations of 3.76-11.28, 0.70-3.48, 0.61-3.06, 0.02-0.08, 0.07-0.36 and 0.07-0.35 μg/mL (r≥0.999 5). The RSD values of precision, repeatability and stability were all less than 2%, and the average sample recovery rates were 102.46%, 101.40%, 102.45%, 102.01%, 102.72%, 101.56%, with RSD below 3% (n=6). Conclusion: The optimized preparation technology is feasible, and the established methods are convenient and reliable. It can be used as the quality control methods for Tongyangxiao Lotion (痛痒消洗剂).

Key words：Tongyangxiao Lotion (痛痒消洗剂); preparation technology; quality standard; TLC; HPLC

发布时间：2026-01-06

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