文献类型：期刊文献

中文题名：贴敷后祖师麻膏药中祖师麻甲素和7-羟基香豆素的残留量测定

英文题名：Determination of residual amounts of daphnetin and 7-hydroxycoumarin in Zushima Plaster used externally

作者：李爽[1];石晓峰[1,2];范彬[2];白朝辉[1]

第一作者：李爽

机构：[1]甘肃中医学院;[2]甘肃省医学科学研究院

第一机构：甘肃中医药大学

年份：2013

卷号：35

期号：6

起止页码：1209

中文期刊名：中成药

外文期刊名：Chinese Traditional Patent Medicine

收录：CSTPCD;;北大核心:【北大核心2011】；CSCD:【CSCD2013_2014】；

基金：甘肃省普通中医药科研课题(GZK-2011-81)

语种：中文

中文关键词：祖师麻膏药;祖师麻甲素;7-羟基香豆素;残留量;高效液相色谱法

外文关键词：Zushima Plaster; daphnetin; 7-hydroxycoumarin; residual amount; HPLC

摘要：目的建立以高效液相色谱法测定祖师麻膏药中祖师麻甲素和7-羟基香豆素的方法,并用于贴敷后祖师麻膏药中药物残留量测定。方法 Agilent Eclipse Plus C18色谱柱(4.6 mm×250 mm,5μm);流动相为乙腈-0.1%磷酸水溶液(15∶85);体积流量为1.0 mL/min;检测波长327 nm。6名健康志愿者签署知情同意书后分别在背部贴敷祖师麻膏药3贴,于24、48、72 h各揭帖1张,采用上述方法测定其祖师麻甲素和7-羟基香豆素的残留量,进而计算残留率。结果祖师麻甲素、7-羟基香豆素的质量浓度分别在16.8～67.2μg/mL(r=0.999 1)、5～60μg/mL(r=0.999 1)范围内与各自峰面积积分值呈良好的线性关系;平均回收率和RSD分别为100.58%、100.53%和1.62%、1.74%(n=9);贴敷24、48、72 h后的祖师麻膏药中祖师麻甲素和7-羟基香豆素的平均残留率分别为69.45%、53.12%、30.00%和93.23%、88.28%、86.74%。结论祖师麻膏药使用后祖师麻甲素和7-羟基香豆素的残留较多,后者更明显存在差异。
AIM To establish an HPLC method for the assay of daphnetin and 7-hydroxycoumarin in Zushima Plaster and their residual amounts used externally.METHODS The determination was performed on Agilent Eclipse Plus column（4.6 mm × 250 mm,5 μm） with mobile phase consisted of acetonitrile and 0.1% phosphoric acid（15∶85） at the flow rate of 1.0 mL/min.The detection wavelength was set at 327 nm.Six healthy volunteers who were signed the informed consent applied three pieces of Zushima Plaster in their backs.The residual amounts of daphnetin and 7-hydroxycoumarin in Zushima Plaster,one piece of which was tore off from each volunteers＇ back in 24,48,72 hours,were determined by HPLC.Then the residual rate was calculated.RESULTS The linear ranges of daphnetin and 7-hydroxycoumarin were 16.8-67.2 μg/mL（r=0.999 1） and 5-60 μg/mL（r=0.999 1）,respectively,and their average recoveries were 100.58%（RSD of 1.62%,n=9） and 100.53%（RSD of 1.74%,n=9）,respectively.The average residual rates of daphnetin and 7-hydroxycoumarin in Zushima Plaster in 24,48,72 h were 69.45%,53.12%,30.00% and 93.23%,88.28%,86.74%,respectively.CONCLUSION HPLC determination shows that the plaster leaves more residual amounts of daphnetin and 7-hydroxycoumarin after being used externally,and the latter is comparatively abundant.