不同产地蒙紫草中左旋紫草素和β,β'-二甲基丙烯酰阿卡宁含量测定及质量标准研究  

Content Determination of L-Shikonin andβ,β’-Dimethylacrylalkannin in Arnebiae Szechenyi Radix from Different Habitats and Study on Its Quality Standard

作　　者：吕晓洁 渠弼 刘德旺 程丹丹 那生桑 LYU Xiaojie;QU Bi;LIU Dewang;CHENG Dandan;NA Shengsang(College of Pharmacy,Inner Mongolia Medical University,Hohhot,Inner Mongolia,China 010110;Mongolian Medicine College of Pharmacy,Inner Mongolia Medical University,Hohhot,Inner Mongolia,China 010110)

机构地区：[1]内蒙古医科大学药学院,内蒙古呼和浩特010110 [2]内蒙古医科大学蒙医药学院,内蒙古呼和浩特010110

出　　处：《中国药业》2021年第17期65-70,共6页China Pharmaceuticals

基　　金：内蒙古自治区人民政府蒙医药标准化项目[2018-[008]];内蒙古自治区自然科学基金[2020LH08026]。

摘　　要：目的建立测定蒙药蒙紫草中左旋紫草素和β,β'-二甲基丙烯酰阿卡宁含量的方法,并制订其质量标准。方法采用显微鉴别法,对药材样品的横切面和粉末进行鉴别;采用薄层色谱法对药材样品中左旋紫草素和β,β'-二甲基丙烯酰阿卡宁进行定性分析;测定药材样品中水分、灰分、浸出物的含量;采用紫外分光光度法测定药材样品中左旋紫草素的含量,检测波长为516 nm;采用高效液相色谱法测定药材样品中β,β'-二甲基丙烯酰阿卡宁的含量,色谱柱为Thermo Hypersil C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.5%甲酸水溶液(70∶30,V/V),流速为1.0 m L/min,检测波长为275 nm,柱温为25℃,进样量为10μL。结果药材样品横切面和粉末显微特征明显;薄层色谱图中可见左旋紫草素和β,β'-二甲基丙烯酰阿卡宁的特征斑点,且斑点分离清晰。左旋紫草素质量浓度在5~50μg/m L(R^(2)=0.9999)范围内与吸光度线性关系良好,β,β'-二甲基丙烯酰阿卡宁的质量浓度在10~200μg/m L(R^(2)=0.9996)范围内与峰面积线性关系良好;精密度、稳定性、重复性试验的RSD均小于2.00%;左旋紫草素和β,β'-二甲基丙烯酰阿卡宁的平均加样回收率分别为101.23%和100.16%,RSD分别为2.01%和2.88%(n=9)。根据1-7号批次药材拟订蒙紫草的质量标准,羟基蒽醌总色素(以左旋紫草素计)含量不得低于1.00%,β,β'-二甲基丙烯酰阿卡宁含量不得低于0.15%;蒙紫草中水分含量不得超过12.00%,总灰分含量不得超过8.00%,酸不溶性灰分含量不得超过2.00%,水溶性浸出物含量不得低于30.00%,醇溶性浸出物含量不得低于10.00%。结论该方法操作简便,结果准确,重复性高,稳定性好,可用于蒙药蒙紫草中左旋紫草素和β,β'-二甲基丙烯酰阿卡宁的含量测定和质量控制。Objective To establish a method for the content determination of L-shikonin andβ,β’-dimethylacrylalkannin in Arnebiae szechenyi Radix,and to formulate its quality standard.Methods The cross-section and powder of medicinal samples were identified by microscopic identification,the L-shikonin andβ,β’-dimethylacrylalkannin in medicinal samples were qualitatively identified by the thin-layer chromatography(TLC)method,the contents of water,ash and extract were determined,and the content of L-shikonin in medicinal samples was determined by ultraviolet spectrophotometry at the detection wavelength of 516 nm.The content ofβ,β’-dimethylacrylalkannin in medicinal material samples was determined by the high-performance liquid chromatography(HPLC)method,the chromatographic column was Thermo Hypersil C18 column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.5%formic acid aqueous solution(70∶30,V/V),the flow rate was 1.0 m L/min,the detection wavelength was 275 nm,the column temperature was25℃,and the injection volume was 10μL.Results The microscopic characteristics of cross-section and powder of the samples were obvious,and the characteristic spots of L-shikonin andβ,β’-dimethylacrylalkannin could be seen in the TLC chromatogram,and the spots were separated.The concentration of L-shikonin showed a good linear relationship with absorbance in the range of 5-50μg/m L(R^(2)=0.9999),and the concentration ofβ,β’-dimethylacrylalkannin showed a good linear relationship with the peak area in the range of 10-200μg/m L(R^(2)=0.9996).The RSDs of precision,stability and repeatability tests were all less than 2.00%.The average recoveries of L-shikonin andβ,β’-dimethylacrylalkannin were 101.23%and 100.16%with RSDs of 2.01%and 2.88%(n=9),respectively.The quality standard of Arnebiae Szechenyi Radix was formulated according to batches 1-7,which was as follows:the content of hydroxyanthraquinone pigments(calculated by L-shikonin)andβ,β’-dimethylacrylalkannin should not be less than 1.00%,0.15%,respec

关 键 词：蒙药 蒙紫草 左旋紫草素 β β'-二甲基丙烯酰阿卡宁 含量测定 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学]