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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
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篇名: 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
TITLE: Comparative Study on the Contents of Four Compounds from Different Processed Products of Miao Medicine Chimonanthus nitens and Its Toxicity
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1mL/min,检测波长为214nm,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、>10000mg/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。
ABSTRACT: 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 10 μL. Modified Karber method was used to determine the LD 50 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 0.019-1.856,0.016-1.616,0.009-0.920,0.006-0.624 μg(R2 were all not lower than 0.999 5). 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 1.119 0%,0.904 3%, 1.068 4%and 0.036 4%;those o f fraxin were 0.867 8%,0.453 9%,0.423 7%and 0.020 5%;those of scopoletin ; those of isofraxidin were 0.110 2%,0.202 1%,0.208 1% and 0.249 4%in samples after drying in the shade ,oven CX-2018-001) drying, steam, charring. The LD 50 of 4 processedproducts were 4 118.13,3 733.36,1 643.61,>10 000 qq.com mg/kg samples ;95%CI were (3 748.87,4 523.76), (3 422.16,4 072.86),(1 520.90,1 776.23),(>10 000) 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. niten s. 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.
期刊: 2020年第31卷第12期
编辑: 王雪,王丽,廖秀,王海波,杨娟,李齐激,杨小生
AUTHORS: WANG Xue,WANG Li,LIAO Xiu,WANG Haibo,YANG Juan,LI Qiji,YANG Xiaosheng
关键字: 铁筷子;炮制;含量;急性毒性;糖苷类成分;小鼠
KEYWORDS: Chimonanthus nitens ;Processing;Content;Acute toxicity ;Glycosides;Mice
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