![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)
3.34 吴茱萸
吴茱萸为芸香科植物吴茱萸Euodia rutaecarpa (Juss.)Benth.、石虎Euodia rutaecarpa (Juss.)Benth. var. officinalis(Dode)Huang或疏毛吴茱萸Euodia rutaecarpa (Juss.)Benth. var. bodinieri(Dode)Huang的干燥近成熟果实,具有散寒止痛、降逆止呕、助阳止泻等功效。现代药理研究表明,吴茱萸碱具有强心、舒张血管、调节血压、松弛胃肠平滑肌、抗肿瘤等作用,其主要活性成分为生物碱类化合物,包括吴茱萸碱、吴茱萸次碱等。
【主要化学成分与结构】
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/b126.jpg?sign=1738843055-2w7WpbD8TBxV9HP2WrqNEkS9i1TK4WMu-0-a116dc03352489265cae9821e57cdd04)
【主要化学成分提取、分离】[48,50]
(1)分离方法一
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file219.png?sign=1738843055-Nnhx1cbkHbO0vlK1cxnF6Gkc2vd22mEL-0-5eb66ea88a408b0fad00d32ed8e18faf)
图3-93 吴茱萸二氯甲烷粗提物的制备HSCCC分离图[48]
HSCCC条件:柱体积125mL;溶剂系统,正己烷-乙酸乙酯-甲醇-水(5∶5∶5∶5),上相作为
固定相,下相作为流动相;转速855r/min;流速2.0mL/min;进样量400mg/10mL;检测波长254nm。
A—柠檬苦素(6.2mg,96.2%);B—吴茱萸碱(10.4mg,98.1%);C—吴茱萸次碱(10.5mg,95.4%)
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file220.png?sign=1738843055-uiB2Z2isGunw0IvxpaoZhUAbX0paxWP8-0-e0598465a0419aa91f0a6efdbaea67fa)
图3-94 吴茱萸二氯甲烷萃取物的HPLC分析图[48]
HPLC条件:Hypersil BDS C18色谱柱(4.6mm×200mm,5μm);紫外检测波长225nm;
柱温,室温;流速1.0mL/min;进样量10μL;流动相,乙腈-水,0~30min,40%~50%乙腈;
30~35min,50%~75%乙腈;35~55min,75%~80%乙腈。1—柠檬苦素;2—吴茱萸碱;
3—吴茱萸次碱;4—1-甲基-2-十一烷基-4(1H)-喹诺酮
(2)分离方法二
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file221.png?sign=1738843055-UC0VgrrRi6IPjwTbMjJalFquV1KzDKvQ-0-c10d5bbca729563717303cdf3817c7e5)
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file222.png?sign=1738843055-tJSNs61SJ9XyUvYDnEsntIbKpik9xdzW-0-ce656d39ebdac3a23934c59c603c8522)
图3-95 吴茱萸粗提物的制备HSCCC分离图[49]
HSCCC条件:柱体积260mL;溶剂系统,正己烷-乙酸乙酯-甲醇-水(5∶5∶7∶5,体积比),
上相作为固定相,下相作为流动相;转速900r/min;流速2mL/min;进样量180mg/4mL;
检测波长254nm;固定相保留率50%。Ⅰ—吴茱萸碱(28mg,98.7%);Ⅱ—吴茱萸次碱
(19mg,98.4%);Ⅲ—吴茱萸新碱(21mg,96.9%);Ⅳ—1-methy-2-[(6Z,9Z)]-
6,9-pentadecadienyl-4-(1H)-quinolone(16mg,98.0%);
Ⅴ—1-methyl-2-dodecyl-4-(1H)-quinolone(12mg,97.2%)
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file223.png?sign=1738843055-3lATWA1U3cjDNGKTIwPyh4bdSSteoNo9-0-fb88326ff6f5d292ccb7d7a9859758f7)
图3-96 吴茱萸粗提物的HPLC分析图[49]
HPLC条件:SPHERIGEL ODS C18色谱柱(4.6mm×250mm,5μm);
紫外检测波长254nm;流速1.0mL/min;流动相,
甲醇-乙腈-水(0~22min,15∶38∶47;22~65min,
45∶38∶17)
(3)分离方法三
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file224.png?sign=1738843055-IvyEQGOuhdMaaY3m5y8M4FJGEworq5On-0-2a9aad4b5ed3be86d51628b86366e5bc)
图3-97
![](https://epubservercos.yuewen.com/C6B5B7/16499754004585606/epubprivate/OEBPS/Images/file225.png?sign=1738843055-bIRpLXV9tUe2dQKodWiHjiG1UgNDqkjE-0-59916a74afcc3105cbaf055f5551961f)
图3-97 吴茱萸粗提物的制备HSCCC分离图(a)及1和2组分的HPLC
分析图(b)及二次HSCCC分离图(c)[50]
HSCCC条件:柱体积250mL;溶剂系统,正己烷-乙酸乙酯-甲醇-水(3∶2∶3∶2)(a);
(12∶8∶11∶8)(c),上相作为固定相,下相作为流动相;转速855r/min;流速2mL/min;
进样量500mg/10mL。1—1-methyl-2-undecyl-4(1H)-quinolone(25.9mg,94.3%);
2—吴茱萸新碱(66.7mg,95.2%);3—1-methy-2-[(6Z,9Z)]-6,9-pentadecadienyl-4-(1H)-
quinolone(29.2mg,96.8%);4—二氢吴茱萸卡品碱(28.0mg,98.3%);5—1-methyl-2-
[(Z)-10-pentadecenyl]-4(1H)-quinolone and 1-methyl-2-[(Z)-6-pentadecenyl]-4(1H)-quinolone
(6.8mg,96.8%)
HPLC条件:Hypersil BDS C18柱(4.6mm×200mm,5μm);检测波长225nm;
柱温25℃;流速1.0mL/min;流动相,乙腈(A)-水(B),0~30min,40%~50%A,
30~35min,50%~75%A,35~55min,75%~80%A,55~60min,80%A