![中药化学成分程序化分离制备](https://wfqqreader-1252317822.image.myqcloud.com/cover/54/29974054/b_29974054.jpg)
3.38 延胡索
延胡索为罂粟科植物延胡索Corydalis yanhusuo W.T.Wang的干燥块茎,具有活血、行气、止痛等功效。现代药理研究表明,延胡索生物碱类成分具有镇痛解痉、活血利气以及对心血管系统的药理作用。其主要活性成分包括延胡索乙素和原阿片碱、脱氢紫堇碱、黄藤素、黄连碱、非洲防己碱等。
【主要化学成分与结构】
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/b137.jpg?sign=1738884761-6OwvpZPUsFs3IuukpP3llsPm1JAhWfCh-0-0c5b58fc049ce0cb83168bb58f2dfce8)
【主要化学成分提取、分离】[55~58]
(1)分离方法一
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file240.png?sign=1738884761-t0HJdQIiQVfahrqjmZCXCD6E3T0gU0Iz-0-5b75755b17e4d2210fd4e5e82ab95028)
图3-107
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file241.png?sign=1738884761-ngVzzAx16VNCj64tj6O6jd0ayibuSA1V-0-835e79ef764b3b6e00ecca8a1eea972b)
图3-107 延胡索粗提物的制备HSCCC分离图[55]
HSCCC条件:柱体积300mL;溶剂系统,石油醚-乙酸乙酯-甲醇-水(22∶25∶23∶17),
上相作为固定相,下相作为流动相;流速2mL/min;进样量100mg。4—原阿片碱
(16.9mg,99.3%);5—延胡索乙素(14.7mg,98.8%)
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file242.png?sign=1738884761-bLt5Bd5s6ikEiRubCHzmiu7BrAvGPkPI-0-62d6f2467fc5547a7f4472fe2f245a1e)
图3-108 延胡索粗提物及HSCCC分离后组分的HPLC分析图[55]
HPLC条件:Agilent C18(4.6mm×150mm,5μm);紫外检测波长280nm;柱温25℃;
进样量10μL;流动相,甲醇-0.1%磷酸缓冲液(三乙胺调pH 6.0)=35∶65
(2)分离方法二
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file244.png?sign=1738884761-n9NVbqF9bbYEJhdZfs7vmx6sBjcJm4xd-0-472c1b254796b29139a4ec8648c4fe03)
图3-109 延胡索粗提物的制备HSCCC分离图[56]
HSCCC条件:柱体积260mL;溶剂系统,四氯化碳-三氯甲烷-甲醇-0.2mol/L盐酸
(1∶7∶3∶4,体积比)(0~150min),氯仿-甲醇0.2mol/L盐酸(7∶3∶4,体积比)
(150~600min),上相作为固定相,下相作为流动相;流速2mL/min;进样量200mg;
固定相保留率57.7%。Ⅰ—未知化合物;Ⅱ—脱氢紫堇碱(27.1mg,99.1%);
Ⅲ—黄藤素(11.5mg,97.1%);Ⅳ—未知化合物;Ⅴ—黄连碱(20.0mg,99.7%);
Ⅵ—非洲防己碱(3.0mg,94.9%)
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file245.png?sign=1738884761-XcHRVbV4ZsBNlE5FRaPpWlrbHZdPmA2G-0-68f21ac6ca2b31c16fa7727977c7040b)
图3-110 延胡索粗提物的HPLC分析图[56]
HPLC条件:Shim-Pack CLC-ODS C18(6mm×250mm,5μm);紫外检测波长345nm;
流速0.6mL/min;流动相,乙腈-0.03mol/L磷酸二氢钾(1.670g SDS/L)=32∶68。
1—脱氢紫堇碱;2—黄藤素;3—黄连碱;4—非洲防己碱
(3)分离方法三
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file246.png?sign=1738884761-qq4bnDxgfcJxjDQPeHrtnriFjoXhdw8o-0-6a4585993373cb6e36439d712df27045)
图3-111 延胡索粗提物的制备HSCCC分离图[57]
HSCCC条件:柱体积220mL;溶剂系统,正己烷-乙酸乙酯-甲醇-水(4∶6∶5∶5),
上相作为固定相,下相作为流动相(6mL样品溶液中加10μL乙酸);紫外检测波长280nm;
转速850r/min;流速1.5mL/min;进样量25mg/6mL;固定相保留率63%。
延胡索乙素(4.37mg,92.7%)
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file247.png?sign=1738884761-W2KyuxteIsvccXOhTDxWTOKdyivheciW-0-6ee48c01923c8c22682261e66cf0efdf)
图3-112 延胡索粗提物的HPLC分析图[57]
HPLC条件:Ultrasphere C18(4.6mm×250mm,5μm);紫外检测波长280nm;流速0.9mL/min;
进样量20μL;流动相,溶剂A[甲醇-水-乙酸-三乙胺(10∶89.1∶0.8∶0.1)],溶剂B
[甲醇-水-乙酸-三乙胺(89.1∶10∶0.8∶0.1)],梯度洗脱:0~10min 1%~16% B,
10~35min 16%~40% B,35~60min 40%~100% B
(4)分离方法四
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file248.png?sign=1738884761-mZkcOYHsZxUp3NHBewEgiYxC8OUMNP47-0-008fbbb5e4d93d0182e423136dc0825f)
图3-113 延胡索粗提物的制备HSCCC分离图[58]
HSCCC条件:溶剂系统,石油醚-乙酸乙酯-甲醇-水(15∶30∶21∶20),上相作为固定相,
下相作为流动相;转速850r/min;检测波长280nm;温度20℃;流速1.2mL/min;进样量200mg;
固定相保留率55.21%。5—延胡索乙素(8.6mg,96.4%)
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file250.png?sign=1738884761-n7T89FfkvB7aB7InT1qEGE0BMddC3Dkr-0-82517e91f8ed5827651930007e076756)
图3-114 延胡索粗提物及HSCCC分离后组分的HPLC分析图[58]
HPLC条件:YMC C18(4.6mm×150mm,5μm);紫外检测波长280nm;流速1mL/min;
进样量20μL;流动相,甲醇-0.1%磷酸(加入二乙胺,pH 6.0)(65∶35,体积比)。
(a)延胡索乙素对照品;(b)延胡索粗提物;(c)HSCCC分离得到的延胡索乙素