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苗药铁筷子不同炮制品中4种成分含量及毒性的比较研究

Comparative Study on the Contents of Four Compounds from Different Processed Products of Miao Medicine Chimonanthus nitens and Its Toxicity
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摘要 目的:比较苗药铁筷子阴干、烘干、蒸制、炒炭制品中4种成分的含量及其毒性。方法:采用高效液相色谱法(HPLC)同时测定铁筷子炮制品中东莨菪苷、秦皮苷、东莨菪内酯、异嗪皮啶的含量。色谱柱为Welch-C18,流动相为乙腈-水(梯度洗脱),流速为1 mL/min,检测波长为214 nm,柱温为30℃,进样量为10μL。采用改良寇氏法测定铁筷子不同加工炮制品对小鼠的半数致死量(LD50)及其95%置信区间(CI),并评价其急性毒性。结果:东莨菪苷、秦皮苷、东莨菪内酯、异嗪皮啶检测质量的线性范围分别为0.019~1.856、0.016~1.616、0.009~0.920、0.006~0.624μg(R2均不低于0.9995),精密度、稳定性、重复性试验的RSD均小于2.0%(n=6);平均加样回收率分别为104.49%、102.22%、101.45%、99.26%(RSD均小于2%,n=6);阴干、烘干、蒸制、炒炭品中,东莨菪苷含量分别为1.1190%、0.9043%、1.0684%、0.0364%,秦皮苷含量分别为0.8678%、0.4539%、0.4237%、0.0205%,东莨菪内酯含量分别为0.0771%、0.1555%、0.0844%、0.2908%,异嗪皮啶含量分别为0.1102%、0.2021%、0.2081%、0.2494%;4种炮制品的LD50分别为4118.13、3733.36、1643.61、>10000 mg/kg,95%CI分别为(3748.87,4523.76)、(3422.16,4072.86)、(1520.90,1776.23)、(>10000)mg/kg。结论:HPLC法重复性、精密度较好,可用于同时测定铁筷子不同炮制品中4种成分的含量;不同炮制品中4种成分均有所差异,2个糖苷类毒性成分的含量明显下降;4种炮制品均为低毒或无毒。 OBJECTIVE:To compare the contents of 4 components and toxicity from Miao medicine Chimonanthus nitens samples after drying in the shade,oven drying,steam,charring.METHODS:The contents of scopolin,fraxin,scopoletin and isofraxin were simultaneously determined by HPLC.The separation was performed on Welch-C18 column with mobile phase consisted of acetonitrile-water(gradient elution)at the flow rate of 1 mL/min.The detection wavelength was set at 214 nm,and column temperature was 30℃,and the sample size was 10μL.Modified Karber method was used to determine the LD50 and its 95%CI of different processed C.nitens to mice and evaluate its acute toxicity.RESULTS:The linear range of scopolin,fraxin,scopoletin and isofraxin were 0.019-1.856,0.016-1.616,0.009-0.920,0.006-0.624μg(R2 were all not lower than 0.9995).RSDs of precision,stability and reprodu-cibility tests were all lower than 2.0%(n=6).The average recoveries were 104.49%,102.22%,101.45%,99.26%(all RSDs were lower than 2%,n=6).The contents of scopolin were 1.1190%,0.9043%,1.0684%and 0.0364%;those of fraxin were 0.8678%,0.4539%,0.4237% and 0.0205%;those of scopoletin were 0.0771%,0.1555%,0.0844%and 0.2908%;those of isofraxidin were 0.1102%,0.2021%,0.2081%and 0.2494%in samples after drying in the shade,oven drying,steam,charring.The LD50 of 4 processed products were 4118.13,3733.36,1643.61,>10000 mg/kg samples;95%CI were(3748.87,4523.76),(3422.16,4072.86),(1520.90,1776.23),(>10000)mg/kg.CONCLUSIONS:HPLC method is reproducible and precise.It can be used to determine the contents of 4 components in different processed products of C.nitens.The contents of 4 components in different processed products,and the contents of glycosides toxicity components are decreased significantly.All the 4 processed products were low or non-toxic.
作者 王雪 王丽 廖秀 王海波 杨娟 李齐激 杨小生 WANG Xue;WANG Li;LIAO Xiu;WANG Haibo;YANG Juan;LI Qiji;YANG Xiaosheng(State Key Laboratory for Efficacy and Utilization of Medicinal Plants,Guizhou Medical University,Guiyang 550014,China;Guizhou Provincial Key Laboratory for Natural Product Chemistry,Chinese Academy of Sciences,Guiyang 550014,China;College of Pharmacy,Guizhou Medical University,Guiyang 550016,China;Sunflower Pharmaceutical Group(Guizhou)Hongqi Co.,Ltd.,Guizhou Liupanshui 553400,China)
出处 《中国药房》 CAS 北大核心 2020年第12期1475-1480,共6页 China Pharmacy
基金 贵州省高层次创新型人才项目(No.黔科合人才〔2015〕4027号) 贵阳市科技计划项目(No.筑科合同〔2017〕8-2号) 贵阳国家高新技术产业开发区管理委员会科技计划项目(No.GXCX-2018-001)。
关键词 铁筷子 炮制 含量 急性毒性 糖苷类成分 小鼠 Chimonanthus nitens Processing Content Acute toxicity Glycosides Mice
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