不同加工方法牡丹皮中7种指标性成分的含量测定及质量评价
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篇名: 不同加工方法牡丹皮中7种指标性成分的含量测定及质量评价
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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10 μL,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0.002~0.034 μg(r=0.999 9)、0.003~0.045 μg(r=0.999 9)、0.013~0.189 μg(r=0.999 8)、0.019~0.291 μg(r=0.999 9)、0.002~0.030 μg(r=0.999 9)、0.050~0.752 μg(r=0.999 9)、0.005~0.076 μg(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,牡丹皮产地加工时可选择“留皮去心药材”“留皮去心鲜切片”两种加工方法。
ABSTRACT: 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 10 μL 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 0.002-0.034 μg(r=0.999 9), 0.003-0.045 μg(r=0.999 9), 0.013-0.189 μg(r=0.999 8), 0.019-0.291 μg(r=0.999 9), 0.002-0.030 μg(r=0.999 9), 0.050-0.752 μg(r=0.999 9) and 0.005-0.076 μg(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 Cortex Moutan that removed both cork and xylem(0.532) > the fresh-cut slice of Cortex Moutan that retained cork but romoved xylem(0.523) > the original medicinal materials of Cortex Moutan that retained cork but removed xylem(0.522) > the fresh-cut slice of Cortex Moutan that removed both cork and xylem(0.502) > the original medicinal materials of Cortex Moutan that removed cork but retained xylem(0.420) > the fresh-cut slice of Cortex Moutan that removed cork but retained xylem(0.409) > the fresh-cut slice of Cortex Moutan that removed both cork and stayed xylem(0.396). As a whole, the quality of the samples of Cortex Moutan which had retained cork was higher than the quality of the samples of Cortex Moutan which had removed cork. CONCLUSIONS: HPLC method is accurate, reliable and repeatable for simultaneous determination of 7 indicator components in Cortex Moutan by different processing methods. Grey correlation degree method can be used for evaluating the quality of Cortex Moutan by different processing methods. The two methods of “fresh-cut slice of Cortex Moutan that retained cork but removed xylem” and “original medicinal materials of Cortex Moutan that retained cork but removed xylem” can be used to process fresh Cortex Moutan in habitats.
期刊: 2018年第29卷第22期
作者: 张洪坤,王其丰,郭长达,吴韶辉,路丽,莫毛燕,高贯彪
AUTHORS: ZHANG Hongkun,WANG Qifeng,GUO Changda,WU Shaohui,LU Li,MO Maoyan,GAO Guanbiao
关键字: 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
KEYWORDS: Cortex Moutan; Field processing; HPLC; Grey correlation degree method; Content determination; Quality evaluation
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