【作者】 聂凌云；

【导师】 吴玉田； 宓鹤鸣； 吴玫涵；

【作者基本信息】 第二军医大学 ， 药物分析学， 2003， 硕士

【摘要】 小茴香不仅是一种常用的调味品，还是一味常用中药，具有温肾散寒、和胃理气功效。本文以小茴香为研究对象，通过对其来源、性状、显微鉴别、薄层色谱鉴别、指纹图谱鉴别、检查、含量测定、气质联用成分分析等多方面的系统分析研究，提出小茴香品质客观评价指标，完善了小茴香的鉴别方法，增加了小茴香药典标准的含量测定项，制定了小茴香药材的进出口国家标准。课题研究主要分三个部分。 第一部分 小茴香研究进展 小茴香始载于《唐本草》，原名怀香，经考证与药典规定的正品(伞形科植物茴香Foeniculum vulgare Mill．的干燥成熟果实)一致。全国大部分地区均有栽培，主产于内蒙、宁夏、山西、新疆等地，有小茴香从东南亚一带进口我国。莳萝、葛缕子、田葛缕子、孜然是小茴香的主要混伪品种，一般通过外观性状、显微鉴别及薄层色谱来加以区分。 小茴香主要含脂肪油、挥发油、甾醇及糖苷、氨基酸等。挥发油是小茴香药材的主要有效成分。炮制有利于挥发油成分的煎出。 小茴香药材具有多方面的药理作用，如对胃肠蠕动的促进，抗溃疡，利胆，中枢麻痹，松弛气管，促进肝恢复和性激素样作用，尤其具有提高免疫、抗肿瘤、杀菌、降压等多种作用。大量应用的毒副作用未见报道。临床应用范围较广，药典及部颁标准收载含小茴香的复方中药品种有68个。 第二部分 小茴香中挥发油成分的质量控制研究 我们共收集了10种不同产地药材小茴香，产地分别为内蒙古托苦托县、山西太原、广东、上海、陕西西安、宁夏、新疆、四川、河北保定、北京。(以上药材经总后药检所中药室刘云主任鉴定均为伞形科植物茴香Foeniculum vulgare Mill．的干燥成熟果实)，进行以下实验研究： 用水蒸气蒸馏法提得各挥发油。采用GC-MS技术建立了小茴香挥发油成分的分析方法：GC：色谱柱为HP-5石英毛细管柱，柱长30cm；内径0.25mm；载气为高纯氦(99.999％)；柱流量为1ml／min；分流比30：1；柱前压8psi：进样口温度250℃；接口温度280℃，进样量1ul。程序升温：柱温50℃(10min)2℃／min 150℃(1min)5℃／min 200℃(5min)。MS：电离方式EI，电子能量70eV，接口温度280℃，离子源温度200℃，四极杆温度100℃，质量扫描范围中文摘要硕士研究论文35一5 0 OAMU，溶剂延迟3.omin。对比各药材的总离子流图，进行了组分差异分析。不同产地小茵香的总离子流图有较大共同点，但亦存在不同之处，各组分的相对百分含量不尽相同。共鉴定出20种化合物，占挥发油总组分的94%以上。其中反式茵香脑(Trans一anethole)的相对含量为65%一78%。 采用毛细管气相色谱法建立了以甲苯为内标的小茵香挥发油中反式茵香脑的含量测定方法:挥发油用二氯甲烷定量溶解稀释后用石英毛细管柱进行气相分析。色谱柱(DB一17 15mX .25oX .25um Temp:40 to 280/3O0oC)，柱温采用程序升温50oC5oC/min 60oC20oC/min200oC(Zmin)，载气为HZ气，检测器FID，内标物为甲苯，分流进样，分流比30:1，进样温度250℃，检测温度250℃。结果:加样平均回收率为97.56%，RSD为1.17%(n=6)。结论:实验结果表明，本方法简便、快速、准确，可用于控制小茵香药材及挥发油的质量。 进行了指纹图谱鉴别方法的初步研究。对比前期所做的各样本用毛细管柱分离后用质谱检测器和用氢火焰检测器检测得到的的总离子流图和色谱图，发现用氢火焰检测的分离色谱图中各成分色谱峰基线分离良好，相对保留时间稳定，精密度、稳定性、重现性均很好，且较质谱检测器应用广泛。故采用气相色谱法初步建立了小茵香药材的指纹图谱。技术参数要求:共有峰的峰号(相对保留时间):1(0 .58)，2(0.62)，3(0.63)，4(0.68)，5(0.72)，6(0.80)，7(0.88)，8(0.96)，S(1.00)，9(1.12)。方法:取供试品溶液lul注入气相色谱仪，记录各峰保留时间和色谱图，应符合以上参数。供试品溶液的制备:精密吸取挥发油测定项下挥发油0.5ml，加二氯甲烷使制成每lml含lul的溶液，做为供试品溶液。对照品溶液的制备:精密称取反式茵香脑对照品10mg，置IOml棕色量瓶中，加二氯甲烷溶解并稀释至刻度，摇匀，作为对照品溶液。仪器与试剂:HEWLETT一PACKARD 5890 SERIES 11型气相色谱仪，迪马公司DB一5[30mX.25nunX.25umTemp:一60 to 325/350(5阶Phenyl)Methylpolysiloxane]石英毛细管柱。反式茵香脑(trans一Anethole)为S工GMA试剂(经归一化法测定其含量为99.9%)，二氯甲烷为分析纯试剂。测定条件:以(5%一苯基)甲基聚硅氧烷共聚物为固定相，涂布厚度0.25um;柱温为程序升温:50’C(lmin)soC/minZO0oC(Zmin)，理论板数按反式茵香脑峰计应不低于5000。 第三部分小茵香新质量标准的制定 从性状、鉴别、检查、含量测定各个方面进行系统分析和相关实验。对原岁中文摘要硕士研究论文药材外观性状对比，横切面、粉末制片镜检显微特征鉴别和最佳薄层色谱条件进行摸索，制定两个显微鉴别和1个薄层色谱鉴别。采用气相色谱法初步建立小茵香指纹图谱鉴别。对小茵香药材中杂质、水分、总灰分、酸不溶性灰分进行考察并规定了合理限度。采用水蒸气蒸馏法提取更多还原

【Abstract】 Fennel is not only a general-adopted flavouring essence, but also a Chinesemedicine of dispelling cold, relieving pain and regulating the stomach function. We mainly aimed at fennel in china area and founded a higher standard of the quality of fennel through a great deal of studies on source, character,identification and the analysis of compositions.The research can be divided into three sections:One section General research work of FennelFennel,as a tranditional Chinese herb used in common,was first recorded in TangPharmacopoeia.Huaixiang was its old name,it is verified the same as the legal goods(Foeniculum vulgare Mill.).It is planted almost all area in china, especially in Inner Mongolia, Ningxia, Shanxi, Xinjiang. There are some imported goods from southeast Asia.Dill,Geluzi,Tiangeluzi, Ziran are the main fake variety.People distinguish them by observing their outside characters or through microscopical identification and thin-layer chromatography .The components of Fennel are fatty oil, volatile oil, sterol, glucoside, amino acid etc. The major component of Fennel is volatile oil. Processing medicine using heat is beneficial for the extracting of volatile oil. There is a little research work on the component of fennel and less report can be found.Fennel has various pharmacodynamical functions, such as promoting to the movement of stomach and intestines, contradicting ulcer, benefitting gallbladder, paralysing center, relaxing trachea, accelerating the resume of liver and hormonelike function, especially have improving immunity resisting tumour sterilizing bacteriunu falling blood pressure and so on. It is not reported for toxicity and side-effect on glut using, proved to be a safe Chinese traditional medicine. It also has a wide range clinical application.There are 68 compound Chinese traditional medicinecontain this herb.Two section Study on the quality control of volatile oilwe totally collect the following 10 breeds of the domestic crude drug. Fennel crude drug yielded respectively by Inner Mongolia Tuokutuo Town, Taiyuan,Guangdong, Shanghai, Xi’an, Ningxia, Xingjiang, Sichuan, Baoding and Beijing. The above crude drugs are proved to be the ripe fruit of Foeniculum vulgare Mill.The chemical components of the volatile oil in the Fennel from 10 areas were analyzed by GC-MS. The essential oil was extracted from fennel by steam distillation, the components analyzed with the different kinds of capillary columns,the optimum separated and analytical conditions were researched,the amount of the components from the essential oil were determinated by normalization method.The components separated were identified by GC-MS.Chromatographic conditions were : Capillary column HP-5(30m 0.25mm,0.25um);Column temperature :50 (10min) , 2/min to 150(lmin), 5/min to 200(5min); Split injection,split ratio 30:l;Injector temperature 250 .Mass spectrum conditions were:ionization mode:EI,Electron energy70eV,Interface temperature:280 Jonicfountain temperature:200 ,quadropole temperature 100, Mass scan range:35-500AMU, Solvent delay 3.0min. There are 20 components composed of above 94% of the total essential oil were separated and identified. The relatively content of trans-anethole was 65%-78%,it might be a quantify character. Analysed and compared their total ion chromatograms(TIC), the TICs are similar, but there is a little different in the TIC and the relative percentage contents. Their similar components may be used in identification of Fructus foeniculi. The method is reliable,stabilize and good repeatability,this method can be applied to the analysis of the essential oil components was extracted from Chinese traditional medicine components.An assay method was developed for the determination of trans-anethole in fennel by programmed -temperature capillary GC. The volatile oil was extracted from Fructus foeniculi by steam distillation and was analyzed with capillary columns: Capillary column DB-17(15m 0.25mm,0.25um Temp:40 to 280/300),Column temperature is elevated by the program: 50, 5/min to 60, 2更多还原