摘要
目的:建立黄花油点草药材的质量标准。方法:参照2015年版《中国药典》方法对药材样品的性状、显微结构进行鉴别,对其水分、灰分及浸出物进行检查;采用薄层色谱法(TLC)对药材样品中槲皮素、烟花苷进行定性鉴别;采用高效液相色谱法测定药材样品中葛根素、对羟基苯甲酸、烟花苷、阿魏酸、槲皮素、山柰酚的含量。结果:性状、显微鉴别具有专属性;槲皮素、烟花苷的TLC图斑点清晰,分离度好,阴性对照无干扰;10批药材样品水分含量范围为0.61%～1.89%,总灰分含量范围为6.28%～8.88%,酸不溶性灰分含量范围为0.76%～1.79%,醇溶性浸出物含量范围为1.31%～2.00%,水溶性浸出物含量范围为9.39%～14.27%。葛根素、对羟基苯甲酸、烟花苷、阿魏酸、槲皮素、山柰酚检测进样量线性范围分别为0.031 92～0.111 7μg(r=0.999 6)、0.085 3～0.298 5μg(r=0.999 5)、0.010 76～0.037 66μg(r=0.999 8)、0.070 08～0.245 3μg(r=0.999 8)、0.058 56～0.205 0μg(r=0.999 4)、0.009 860～0.033 88μg(r=0.999 4);定量限分别为1.06、0.47、0.75、1.40、1.20、0.74 ng,检测限分别为0.36、0.12、0.30、0.53、0.60、0.31 ng;精密度、稳定性、重复性试验的RSD均小于2%;平均加样回收率分别为101.54%、102.10%、101.46%、103.35%、99.36%、96.85%,RSD分别为1.76%、1.68%、1.56%、1.26%、0.91%、1.96%(n=6);样品含量分别为0.017～0.047、0.042～0.140、0.003 8～0.015 0、0.049～0.180、0.024～0.091、0.003 9～0.011 0 mg/g。结论:所建质量标准可用于黄花油点草的质量控制。
OBJECTIVE:To establish the quality standard of Tricyrtis maculata. METHODS:The character and microstructure of T. maculata were identified according to the method stated in 2015 edition of Chinese Pharmacopoeia. The contents of moisture, ash and extract were determined. TLC was used for qualitative identification of quercetin and nicotifiorin in samples. The contents of puerarin,p-hydroxybenzoic acid,nicotiflorin,ferulic acid,quercetin and kaempferol were determined by HPLC. RESULTS: The characters and microscopic identification had specificity. TLC spots of quercetin and nicotifiorin were clear and well-separated without interference from negative control. The water content,total ash content,acid insoluble ash content,alcohol soluble extract and water soluble extract for 10 batches of samples were 0.61%-1.89%,6.28%-8.88%,0.76%-1.79%,1.31%-2.00% and 9.39%-14.27%,respectively. The linear range of puerarin,p-hydroxybenzoic acid,nicotiflorin,ferulic acid,quercetin and kaeniphenol were 0.031 92-0.111 7 μg(r=0.999 6),0.085 3-0.298 5 μg(r=0.999 5),0.010 76-0.037 66 μg(r=0.999 8),0.070 08- 0.245 3 μg(r=0.999 8),0.058 56-0.205 0 μg(r=0.999 4),0.009 860-0.033 88 μg(r=0.999 4),respectively. The quantitation limits were 1.06,0.47,0.75,1.40,1.20,0.74 ng,and the detection limits were 0.36,0.12,0.30,0.53,0.60,0.31 ng, respectively. RSDs of precision,stability and repeatability tests were all less than 2%. The average recoveries were 101.54%, 102.10%,101.46%,103.35%,99.36% and 96.85%,respectively;RSDs were 1.76%,1.68%,1.56%,1.26%,0.91% and 1.96%,respectively (n=6);the results of the content were 0.017-0.047,0.042-0.140,0.003 8-0.015 0,0.049-0.180,0.024- 0.091,0.003 9-0.011 0 mg/g. CONCLUSIONS:The established quality standard can be used for the quality control of T. maculata.
作者
任丽
贾田芊
李兴欢
谢晓林
谢晓峰
张德柱
孙静
REN Li;JIA Tianqian;LI Xinghuan;XIE Xiaolin;XIE Xiaofeng;ZHANG Dezhu;SUN Jing(College of Pharmacy,Shaanxi University of TCM,Shaanxi Xianyang 712046,China;Shaanxi Panlong Pharmaceutical Group Co.,Ltd.,Xi’an 710025,China)
出处
《中国药房》
CAS
北大核心
2019年第8期1083-1090,共8页
China Pharmacy
基金
陕西省科技统筹创新工程计划项目(No.2016KTCQ-03-13)
陕西省中医管理局中医药科研课题(No.15-ZY001)
