蒙药乌日格斯图-阿日查(刺柏叶)的质量标准提升
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篇名: 蒙药乌日格斯图-阿日查(刺柏叶)的质量标准提升
TITLE: Improvement of Quality Standard for Mongolian Medicine Juniperus rigida
摘要: 目的:为完善蒙药乌日格斯图-阿日查(刺柏叶)的质量标准提供科学依据。方法:以不同采集地的10批乌日格斯图-阿日查药材为样品,对其进行性状观察和显微鉴别;采用薄层色谱法(TLC)对样品中的异槲皮苷、槲皮苷、穗花杉双黄酮、竹柏双黄酮A和扁柏双黄酮进行定性鉴别;参照2020年版《中国药典》(四部)通则中的相关方法测定样品中总灰分、酸不溶性灰分、醇溶性浸出物、重金属的含量;建立高效液相色谱法(HPLC)测定样品中上述5种成分的含量。结果:乌日格斯图-阿日查粉末呈绿色或黄绿色,管胞呈多角形,紧密排列成纵行;气孔为不等式;表皮细胞为近长方形;厚壁细胞呈类长方形,壁连珠状增厚。TLC结果显示,供试品在与上述5种成分对照品色谱相应位置上显相同颜色的斑点。10批样品中总灰分、酸不溶性灰分、醇溶性浸出物含量分别为7.37%~11.18%、0.75%~2.98%、16.55%~26.42%,平均值分别为8.51%、1.27%、22.35%;铅、砷、镉、汞、铜含量分别为2.00~5.44、0.65~1.65、0.044~0.100、0.034~0.160、4.59~6.79mg/kg,平均值分别为3.73、0.97、0.078、0.061、5.23mg/kg。异槲皮苷、槲皮苷、穗花杉双黄酮、竹柏双黄酮A、扁柏双黄酮检测质量浓度的线性范围分别为4.98~20.02、49.99~199.96、19.94~99.96、9.99~40.00、20.20~159.98μg/mL(r均大于0.9997);精密度、重复性、稳定性(24h)试验的RSD均小于3.00%(n=6);平均加样回收率为100.62%~102.96%,RSD为1.21%~1.88%(n=6)。10批样品中上述5种成分的平均含量分别为0.089~0.379、1.379~4.250、1.077~2.026、0.162~0.423、0.0169~0.1170mg/g。结论:本研究建立了蒙药乌日格斯图-阿日查药材的定性、定量分析方法,暂规定其总灰分不得超过10.22%,酸不溶性灰分不得超过1.53%,醇溶性浸出物不得低于17.88%,重金属铅不得超过5mg/kg,砷不得超过2mg/kg,镉不得超过0.3mg/kg,汞不得超过0.2mg/kg,铜不得超过20mg/kg。
ABSTRACT: OBJECTIVE:To provide scientifi c evidence for improving the quality standard of Mongolian medicine Juniperus rigida. METHODS :Totally 10 batches of J. rigida from different places were taken as samples to observe their characters and identify them by microscope ;TLC method was adopted to qualitatively identify isoquercitrin ,quercitrin,amentoflavone, podocarpusflavone A and hinokiflavone ;the contents of total ash ,acid-insoluble ash ,ethanol-soluble extract and heavy metals were determined by related method stated in 2020 edition of Chinese Pharmacopeia (part Ⅳ). The contents of above 5 components in samples were determined by HPLC. RESULTS :The powder of J. rigida was green or yellowish green ,polygonal tracheids , closely arranged in longitudinal with unequal stomatal ;epidermal cells were nearly rectangular ;sclerenchyma cells were quasi rectangular and the wall beadedly thickening. Results of TLC showed that the spots of the same color were found in the corresponding positions of chromatogram for test sample and substance control. The contents of total ash ,acid-insoluble ash and ethanol-soluble extract in 10 batches of samples were 7.37%-11.18%,0.75%-2.98%,16.55%-26.42%,respectively;average contents were 8.51%,1.27%,22.35%. The contents of lead ,arsenic,cadmium,mercury and copper were 2.00-5.44,0.65-1.65, 0.044-0.100,0.034-0.160,4.59-6.79 mg/kg,respectively;average conte nts were 3.73,0.97,0.078,0.061,5.23 mg/kg. The linear ranges of isoquercitrin ,quercitrin,amentoflavone,podocarpus- flavone A and hinokiflavone were 4.98-20.02,49.99-199.96, 19.94-99.96,9.99-40.00,20.20-159.98 μg/mL(all r>0.999 7); com RSDs of precision ,repeatability and stability (24 h) tests were all less than 3.00%(n=6);the average recoveries were 话:0993-2057878。E-mail:Tanghuishz@qq.com 100.62%-102.96%,RSDs were 1.21%-1.88%(n=6). Average contents of the above-mentioned 5 compounds in 10 batches of samples were 0.089-0.379,1.379-4.250,1.077-2.026,0.162-0.423, 0.016 9-0.117 0 mg/g,respectively. CONCLUSIONS :The qualitative and quantitative analysis methods of Mongolian medicine J. rigida are established. It is preliminarily proposed that the total ash content shall not exceed 10.22%,the acid-insoluble ash content shall not exceed 1.53%,ethanol-soluble extract content shall not be less than 17.88%,heavy metal lead should not exceed 5 mg/kg,arsenic should not exceed 2 mg/kg,cadmium should not exceed 0.3 mg/kg,mercury should not exceed 0.2 mg/kg,copper should not exceed 20 mg/kg.
期刊: 2021年第32卷第16期
作者: 袁小红,庞克坚,唐辉,张虹,管辉,魏沣,唐萍
AUTHORS: YUAN Xiaohong ,PANG Kejian ,TANG Hui,ZHANG Hong,GUAN Hui,WEI Feng,TANG Ping
关键字: 蒙药;乌日格斯图-阿日查;质量标准;薄层色谱法;高效液相色谱法;槲皮苷;穗花杉双黄酮;竹柏双黄酮A
KEYWORDS: Mongolian medicine ; Juniperus rigida ; Quality standard ; TLC;HPLC;Quercitrin;Amentoflavone;
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