摘要
目的:建立同时测定不同加工方法牡丹皮中7种指标性成分含量的方法,并评价其质量。方法:采用高效液相色谱法(HPLC)测定不同加工方法牡丹皮中7种指标性成分的含量,色谱柱为ZORBAX Eclipse XDB-C18,流动相为甲醇-0.1%磷酸溶液(梯度洗脱),检测波长为230、258 nm,流速为1 mL/min,进样量为10μL,柱温为30℃。按《中国药典》的方法测定醇溶性浸出物的含量。采用灰色关联度法以7种指标性成分及醇溶性浸出物含量为指标,以相对关联度为测度,构建牡丹皮药材/饮片质量评价模型并进行质量评价。结果:没食子酸、儿茶素、氧化芍药苷、芍药苷、苯甲酸、丹皮酚、苯甲酰芍药苷的进样量线性范围分别为0.002～0.034μg(r=0.999 9)、0.003～0.045μg(r=0.999 9)、0.013～0.189μg(r=0.999 8)、0.019～0.291μg(r=0.999 9)、0.002～0.030μg(r=0.999 9)、0.050～0.752μg(r=0.999 9)、0.005～0.076μg(r=0.999 8);定量限分别为1.213、1.380、1.307、1.178、0.275、1.538、0.870 ng,检测限分别为0.364、0.414、0.392、0.354、0.083、0.461、0.261 ng;精密度、稳定性、重复性试验的RSD均小于3%;加样回收率分别为101.00%～105.20%(RSD=1.69%,n=6)、96.01%～104.14%(RSD=2.77%,n=6)、93.60%～99.87%(RSD=2.15%,n=6)、95.84%～97.39%(RSD=0.61%,n=6)、95.74%～99.31%(RSD=1.45%,n=6)、98.65%～100.80%(RSD=0.69%,n=6)、100.87%～107.07%(RSD=2.44%,n=6)。不同加工方法牡丹皮的相对关联度范围为0.396～0.590,质量高低排序依次为留皮留心药材(0.590)>去皮去心药材(0.532)>留皮去心鲜切片(0.523)>留皮去心药材(0.522)>留皮留心鲜切片(0.502)>去皮留心药材(0.420)>去皮留心鲜切片(0.409)>去皮去心鲜切片(0.396),留皮药材/饮片样品质量整体优于去皮药材/饮片样品。结论:HPLC法准确、可靠、重复性好,可用于同时测定不同加工方法牡丹皮中7种指标性成分的含量;灰色关联度法可用于评价不同加工方法牡丹皮的质量,牡丹皮产地加工�
OBJECTIVE:To establish a method for simultaneous determination of 7 indicator components in Cortex Moutan by different processing methods,and to evaluate the quality of them.METHODS:HPLC method was adopted to determine the contents of 7 indicator components in Cortex Moutan by different proessing methods.The determination was performed on ZORBAX Eclipse XDB-C18 column with mobile phase consisted of methanol-0.1%phosphoric acid solution(gradient elution)at the flow rate of 1 mL/min.The detection wavelengths were set at 230 and 258 nm.The sample size was 10μL and the column temperature was 30℃.The content of ethanol-soluble extract was determined by the method included in Chinese Pharamacopoeia.The quality evaluation model of Cortex Moutan material/decoction piece was established using 7 kinds of indicator components and ethanol-soluble extract as evaluation index,relative correlation degree as measurement.The quality of Cortex Moutan was evaluated.RESULTS:The linear range of gallic acid,catechin,oxidation paeoniflorin,paeoniflorin,benzoic acid,paeonol and enzoyl paeoniflorin were 0.002-0.034μg(r=0.999 9),0.003-0.045μg(r=0.999 9),0.013-0.189μg(r=0.999 8),0.019-0.291μg(r=0.999 9),0.002-0.030μg(r=0.999 9),0.050-0.752μg(r=0.999 9)and 0.005-0.076μg(r=0.999 8).The limits of quantitation were 1.213,1.380,1.307,1.178,0.275,1.538,0.870 ng,respectively.The detection limits were 0.364,0.414,0.392,0.354,0.083,0.461,0.261 ng,respectively.RSDs of precision,stability and repeatability test were all less than 3%.The recovery rates were 101.00%-105.20%(RSD=1.69%,n=6),96.01%-104.14%(RSD=2.77%,n=6),93.60%-99.87%(RSD=2.15%,n=6),95.84%-97.39%(RSD=0.61%,n=6),95.74%-99.31%(RSD=1.45%,n=6),98.65%-100.80%(RSD=0.69%,n=6),101.87%-107.07%(RSD=2.44%,n=6),respectively.The relative correlation of Cortex Moutan by different processing method was 0.396-0.590.The order of the quality of all processed samples was:the original medicinal materials of Cortex Moutan that retained both cork and xylem(0.590)>the original medicinal materials of C
作者
张洪坤
王其丰
郭长达
吴韶辉
路丽
莫毛燕
高贯彪
ZHANG Hongkun;WANG Qifeng;GUO Changda;WU Shaohui;LU Li;MO Maoyan;GAO Guanbiao(Bozhou Huqiao Pharmaceutical Co.,Ltd.,Anhui Bozhou 236800,China;Guangzhou Xiangxue Pharmaceutical Co.,Ltd.,Guangzhou 510663,China;Shaoguan Food and Drug Inspection Institute,Guangdong Shaoguan 512026,China)
出处
《中国药房》
CAS
北大核心
2018年第22期3063-3068,共6页
China Pharmacy
基金
国家中医药管理局中药标准化项目(No.国中医药办科技函[2016]154号)
国家中医药管理局中药重点产品行业标准制定计划项目(No.国中医药法监函[2017]17号-ZYY-2017-062)
关键词
牡丹皮
产地加工
高效液相色谱法
灰色关联度法
含量测定
质量评价
Cortex Moutan
Field processing
HPLC
Grey correlation degree method
Content determination
Quality evaluation
