产地加工炮制一体化对川芎饮片化学成分的影响研究
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篇名: 产地加工炮制一体化对川芎饮片化学成分的影响研究
TITLE: Study on the Effects of the Integration of Field Processing and Decoction Piece Processing on Chemical Com- position of Ligusticum chuanxiong Decoction Pieces
摘要: 目的:探讨产地加工与饮片炮制一体化(以下简称“一体化”)对川芎饮片化学成分的影响。方法:收集四川都江堰、彭州两地的鲜川芎,除去杂质和非药用部位后,经淋洗、阴干(至含水量约28%)、切片、干燥制得川芎一体化饮片;经阴干、加水闷润(至透心)、切片、干燥制得传统饮片。建立两种饮片各10批样品的高效液相色谱(HPLC)指纹图谱,色谱柱为WondaSilC18,流动相为1%甲酸水溶液-乙腈(梯度洗脱),流速为1.0mL/min,柱温为30℃,检测波长为285nm,进样量为10μL。以洋川芎内酯A为参照,绘制20批药材样品的HPLC指纹图谱;采用《中药色谱指纹图谱相似度评价系统(2004A版)》进行相似度评价,确定共有峰。按上述色谱条件测定两种饮片中绿原酸、阿魏酸、洋川芎内酯A的含量,采用单因素方差分析进行组间比较。结果:20批药材样品HPLC指纹图谱的相似度均大于0.900;共有16个共有峰,指认其中7个依次为绿原酸、阿魏酸、洋川芎内酯Ⅰ、阿魏酸松柏酯、洋川芎内酯A、正丁基苯酞、藁本内酯。绿原酸、阿魏酸、洋川芎内酯A检测质量浓度的线性范围分别为0.008~0.200mg/mL(r=0.9999)、0.010~0.140mg/mL(r=0.9992)、0.100~0.600mg/mL(r=0.9993);定量限分别为0.0028、0.0006、0.0050mg/mL,检测限分别为0.0008、0.0001、0.0010mg/mL;精密度、重复性、稳定性试验的RSD均小于3%,平均加样回收率为96.27%~102.02%(RSD<2%,n=6)。川芎一体化饮片和传统饮片中上述成分的含量分别为(1.6770±0.3110)、(1.5627±0.1245)、(9.4940±1.3513)mg/g和(1.3002±0.4692)、(1.3880±0.2099)、(9.8117±1.0989)mg/g,组间比较差异均无统计学意义(P>0.05)。结论:川芎一体化饮片和传统饮片各批样品化学成分的一致性好,且一体化加工不影响饮片中绿原酸、阿魏酸、洋川芎内酯A等指标性成分的含量,该工艺具有一定的可行性。
ABSTRACT: OBJECTIVE:To investigate the effects of the integration of field processing and decoction piece processing (hereinafter called “Integration”for short )on chemical composition of Ligusticum chuanxiong decoction pieces. METHODS :Fresh L. chuanxiong were collected from Dujiangyan and Pengzhou of Sichuan ;integrated decoction pieces of L. chuanxiong were prepared after washing ,drying in the shade (to about 28% moisture content ),slicing and drying ;traditional decoction pieces was prepared after drying in the shade ,adding water to moisten (to the core ),slicing and drying. HPLC fingerprints of two kinds of decoction pieces samples (with 10 batches in each type )were established. The determination was performed on WondaSil C 18 column with mobile phase consisted of 1% formic acid solution-acetonitrile (gradient elution )at the flow rate of 1.0 mL/min. The column temperature was 30 ℃. The detection wavelength was set at 285 nm,and the sample size was 10 μL. Using ligusticolide A as reference ,HPLC fingerprints of 20 batches of samples were drawn. The similarity of the fingerprints was evaluated with Similarity Evaluation System for Chromatographic Fingerprint of TCM (2004A edition ),and then common peaks were confirmed. The contents of chlorogenic acid ,ferulic acid and ligusticolide A were determined by above chromatographic condition. Single factor variance analysis was performed for comparison of the contents. RESULTS :The similarity of HPLC fingerprints among 20 batches of samples was above 0.900. A total of 16 common peaks were determined ,7 of which were chlorogenic acid ,ferulic acid,ligusticolide Ⅰ,pine cypress ferulinate ,ligusticolide A ,n-butylphthalide and ligustilide ,respectively. The linear range of chlorogenic acid ,ferulic acid and ligusticolide A were 0.008-0.200 mg/mL(r=0.999 9),0.010-0.140 mg/mL(r=0.999 2)and 0.100-0.600 mg/mL(r=0.999 3);the limits of quantification were 0.002 8,0.000 6 and 0.005 0 mg/mL,respectively;the limits of detection were 0.000 8,0.000 1 and 0.001 0 mg/mL,respectively;RSDs of precision ,reproducibility and stability tests were all lower than 3%,and average recoveries were 96.27%-102.02%(RSD<2%,n=6). The contents of above compositions in the integrated decoction pieces and traditional decoction pieces were(1.677 0±0.311 0),(1.562 7±0.124 5),(9.494 0±1.351 3)mg/g and(1.300 2±0.469 2),(1.388 0±0.209 9),(9.811 7±1.098 9)mg/g,respectively;there was no statistical significance between 2 groups(P>0.05). CONCLUSIONS :The chemical composition of each batch of samples of L. chuanxiong integrated decoction pieces and traditional decoction pieces is consistent ,and the content of index components as chlorogenic acid ,ferulic acid and ligusticolide A in the decoction pieces is not affected by the integration processing. This process is feasible to a certain extent.
期刊: 2020年第31卷第06期
作者: 吴情梅,刘晓芬,连艳,陈玲,黄凤,彭成,杨晨,黄维,蒋桂华
AUTHORS: WU Qingmei,LIU Xiaofen,LIAN Yan,CHEN Ling,HUANG Feng,PENG Cheng,YANG Chen,HUANG Wei,JIANG Guihua
关键字: 川芎;一体化饮片;传统饮片;指纹图谱;含量测定;高效液相色谱法
KEYWORDS: Ligusticum chuanxiong ; Integrated decoction piece ; Traditional decoction piece ; Fingerprint; Content
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