液质联用法测定吴茱萸碱、吴茱萸次碱、去氢吴茱萸碱在大鼠脑脊液和脑组织中的分布

吴茱萸碱、吴茱萸次碱、去氢吴茱萸碱是吴茱萸中主要的生物碱类成分.为研究吴茱萸主要生物碱成分在大鼠脑脊液中的代谢和在脑组织中的分布,吴茱萸碱、吴茱萸次碱、去氢吴茱萸碱以1∶1∶1的质量比混合,以15 mg/kg的剂量灌胃给予大鼠.本文建立了同时测定大鼠脑脊液和脑组织中三个生物碱成分的液质联用方法,测定结果显示,三个生物碱...     

薄层荧光扫描法测定吴茱萸药材及其制剂中5种生物碱的含量

目的：用薄层荧光扫描法测定吴茱萸及加味左金丸中5种生物碱:羟基吴茱萸碱(hydroxyevodiamine, I)、N-甲酰二氢吴茱萸次碱(N-formyldihydrorutaecarpine, II)、吴茱萸酰胺甲(goshuyuamide-I, III)、吴茱萸碱（evodiamine, IV)及吴茱萸次碱(rutaecarpine, V)。方法：在高效硅胶薄层板上点样后,二次展开。展开剂:（1）氯仿—石油醚—甲醇—环己烷（5∶3∶0.4∶0.4）;(2)氯仿—甲醇(4.1∶0.3)。展开后用浓盐酸衍生化,荧光扫描测定。结果：各生物碱的线性范围在20.5～245 ng,回收率为96.8%～104.5%,并用此法测定了不同产地吴茱萸及不同批号的加味左金丸中生物碱的含量。结论：方法灵敏度高、样品用量少,可为寻找和利用植物资源,控制生药及方剂质量提供科学依据。     

中药超微饮片的成分组成与原药材成分的差异分析

目的分析中药超微饮片与原药材成分组成的差异性。方法取黄连超微饮片与黄连原药材及盐酸小檗碱标准品。提取并测定两种饮片总生物碱溶出量,采用薄层色谱法定性,高效液相色谱法定量。观察硅胶G薄层板上的斑点。测定并比较盐酸小檗碱含量和总生物碱的溶出量及溶出速度。结果总生物碱溶出量:超微饮片是原药材的1.73倍,浸泡时间短。薄层色谱法:黄连的超微饮片、原药材提取物与盐酸小檗碱标准品在硅胶G板的相同位置有相同颜色的斑点。且超微饮片提取物的颜色较深。高效液相色谱法:黄连的超微饮片提取物的峰面积是原药材提取物的峰面积的1.52倍。两种饮片总生物碱与盐酸小檗碱的含量比较,P<0.05,均具有统计学意义。结论黄连超微饮片于原药材不仅在成分上不存在差异,但是有效成分的溶出效果更好,更利于提取。     

不同采收期对吴茱萸品质的影响

目的考察吴茱萸不同采收期的主要成分的差异,为吴茱萸药材合理利用提供参考。方法应用HPLC方法测定吴茱萸果实中吴茱萸内酯、吴茱萸碱和吴茱萸次碱的含量,以此为指标考察不同采收期药材主要成分的变化规律。结果吴茱萸品种随成熟期不同,生物碱含量呈先升高、再保持稳定、最后随药材的老熟而呈降低的趋势。结论湖南浏阳地区吴茱萸的最佳采收期是8月底,湖南浏阳地区石虎的最佳采收期是9月初,广西柳城地区疏毛吴茱萸的最佳采收期是8月中下旬,广西桂林地区疏毛吴茱萸的最佳采收期是8月中旬。     

薄层扫描法测定夏天无眼药水中原阿片碱的含量

夏天无眼药水为夏天无药材提取的总生物碱加工制成的滴眼剂 ,其主要和有效成分是原阿片碱等生物碱[1] ,具有通络、活血和解除眼睫肌痉挛功效[2 ,3] 。该品种原收载于江西省药品标准 ( 1982年版 ) ,采用雷氏盐 -比色法测定其中总生物碱含量[4 ] ,在生产和检验中发现该方法操作繁琐 ,专属性不强 ,且有一定的误差。卫生部药品标准采用薄层 -紫外法测定原阿片碱的含量[5] 。本文用薄层扫描法对夏天无眼药水中原阿片碱进行含量测定。经大量试验摸索 ,通过优选 ,结果表明 :拟定方法可靠 ,操作简便 ,可作为质量控制方法。1　仪器与试药日本岛津ＣＳ…     

~(60)Co-γ射线辐照贮藏对川贝母质量的影响

目的:研究~(60)Co-γ射线辐照贮藏对川贝母质量的影响。方法:对不同剂量~(60)Co-γ射线辐照处理过的川贝母的霉变、虫蛀情况进行观察,并对辐照和未辐照川贝母的总生物碱和水溶性核苷类成分进行含量比较。结果:经辐照后的川贝母的化学成分、感观形态无明显变化,能有效地防止霉变和虫蛀,明显延长药材的贮藏期;川贝母辐照前后总生物碱和水溶性核苷类成分无含量显著变化。结论:应用~(60)Co-γ射线辐照灭菌杀虫工艺可为富含淀粉及贵重中药材的贮藏提供有效方法。     

制川贝母质量标准研究

目的:建立制川贝母的质量标准。方法:参照2010年版《中国药典》川贝母质量标准中相关方法,建立制川贝母显微鉴别、薄层鉴别、水分测定、总灰分测定、浸出物测定,以西贝母碱为指标的总生物碱含量项目的检查方法并规定限度,采用HPLC法建立制川贝母中贝母辛含量测定方法并拟定含量限度,以此对制川贝母进行质量标准研究。结果:川贝母炮制前后显微鉴别特征变化不大,薄层鉴别显示炮制品和生品提取物没有太大差别,制川贝母的水分不应超过13.0%,总灰分不得超过1.60%,浸出物不得少于25.0%,总生物碱含量以西贝母碱计不得少于0.04%,贝母辛含量不得少于0.02%。结论:本研究可为制川贝母的质量标准的建立提供参考。     

不同产地哈萨克药材白喉乌头中总生物碱含量的分析

目的测定不同产地白喉乌头所含总生物碱的含量。方法采用索式提取法对药材进行提取,结合酸溶碱沉和萃取的方法从药材中提取白喉乌头总生物碱;利用紫外光谱对经过酸性染料络合的生物碱进行分析,检测其中总生物碱的含量。结果新源县、巩留县和昭苏县所产白喉乌头原药材中含有总生物碱分别为2.246,4.682和3.597 mg.g 1;回归方程为Y=11.5X+0.121,r=0.999 6,乌头碱浓度在6～36μg.mL 1内呈良好的线性关系。结论采用紫外-可见分光光度法测定不同产地白喉乌头中总生物碱的含量,具有操作简便、结果准确的特点;其结果可为该药材的活性和毒性物质基础研究提供依据。     

宽筋藤总生物碱含量测定方法研究

目的建立宽筋藤药材中总生物碱的含量测定方法。方法以盐酸药根碱为对照品,采用紫外-可见分光光度法测定宽筋藤总生物碱的含量,测定波长为430nm。结果盐酸药根碱在0.001 1~0.006 5mg·mL-1范围内与吸光度呈良好线性关系,回归方程:Y=14.747 X-0.010 7(r=0.999 5)。盐酸药根碱平均回收率为100.4%,RSD=2.0%(n=6)。结论 16批宽筋藤药材总生物碱含量测定结果表明,所建立的方法简便、准确,可用于宽筋藤药材总生物碱的含量测定。     

萸黄连饮片“反制”前后物质基础差异性研究

目的:从成分差异性角度分析炮制前后萸黄连饮片中多种有效成分的含量变化,初步探讨萸黄连饮片以热制寒的药性差异性的物质基础。方法:采用HPLC-DAD法检测并比较黄连饮片和萸黄连饮片中原小檗碱型生物碱类成分及含量,以及吴茱萸饮片、炮制辅料吴茱萸汁、萸黄连饮片中酚酸类、苦味素类和生物碱类组分中代表性成分及含量,阐述萸黄连饮片反制前后药性相关物质基础差异性。结果:黄连饮片中盐酸小檗碱、盐酸巴马汀、盐酸黄连碱、盐酸药根碱的含量分别为91.62,16.12,46.90,11.40 mg.g-1;萸黄连饮片中盐酸小檗碱、盐酸巴马汀、盐酸黄连碱、盐酸药根碱的含量分别为91.74,16.53,46.66,11.36 mg.g-1;吴茱萸饮片中绿原酸、吴茱萸内酯、吴茱萸碱、吴茱萸次碱的含量分别为10.56,21.56,3.54,3.12 mg.g-1;炮制辅料吴茱萸汁中绿原酸、吴茱萸内酯、吴茱萸碱、吴茱萸次碱的含量分别为6.64,8.23,0.41,0.38 mg.g-1;萸黄连饮片中绿原酸、吴茱萸内酯、吴茱萸碱、吴茱萸次碱的含量分别为3.37,1.49,0.12,0.12 mg.g-1。结论:炮制后萸黄连饮片中黄连饮片本身所含...     

吴茱萸饮片炮制研究进展

本文总结了吴茱萸近几年的炮制研究进展,主要是吴茱萸的产地、采收与有效成分的关系、吴茱萸的炮制工艺研究以及炮制前后的毒性变化研究。作者认为,吴茱萸炮制品中挥发油和生物碱应有控制标准,对于吴茱萸的炮制研究既要进行GAP规范化研究,又要根据中医辨证施治的原则,结合古今炮制经验,通过化学、药理、毒理研究和临床验证,筛选出中药的最佳炮制方法。     

中药吴茱萸中生物碱类成分的HPLC指纹图谱

目的研究中药吴茱萸中生物碱类成分的HPLC特征指纹图谱。方法应用HPLC法分析吴茱萸药材生物碱类成分色谱图。色谱柱:Agilent Extend C18柱(250 mm×4.6 mm,5μm);流动相:乙腈-水系(水-四氢呋喃-乙酸,体积比48∶1∶0.1);洗脱方式:线性梯度洗脱;柱温:35℃;流速:1 mL.min-1;检测波长:240 nm;进样量:20μL。理论板数按吴茱萸次碱计算不低于3 000。结果10批不同来源的吴茱萸药材所含生物碱类成分均得到很好的分离,获得14个共有特征峰。结论HPLC指纹图谱法能较好地识别吴茱萸药材,为吴茱萸的质量控制提供了方法学依据。     

On the evaluation of the preparation of Chinese medicinal prescriptions. VI. The changes of the alkaloid contents by processing of Evodia fruit]

A crude drug, Evodia fruit (goshuyu) was processed to detoxicate and reduce the bitter taste. Following the procedure described in Shokanron, Evodia fruit was washed in hot water, and then dried. The alkaloid contents of processed Evodia fruit was analyzed by high performance liquid chromatography. The result shows that the content of hydroxyevodiamine decreased to 0.55 times, while the content of rutaecarpine and evodiamine hardly change in the final processed material. However, evocarpine content increased to 1.3 times comparing with the untreated Evodia fruit. The phenomena was ascribed to the flowing-out of the water-soluble portion, and also the weight of extract and the intense of bitterness in the processed fruit were reduced to about 1/3 times.     

不同比例黄连-吴茱萸配方颗粒/单/合煎对比分析

目的： 通过考察不同比例的黄连与吴茱萸药对,其配方颗粒与单煎液、合煎液的关键成分含量差异,探索药对配方颗粒与传统煎法的等效性。方法： 采用高效液相色谱法测定不同制法下6种生物碱含量,并利用SPSS18.0进行统计检验。结果： 与单煎相比,配方颗粒中4种黄连生物碱和吴茱萸次碱含量均与合煎中没有明显差异（小檗碱P=0.881;表小檗碱P=0.810;黄连碱P=0.961;巴马汀P=0.220;吴茱萸次碱P=0.137）,单煎中黄连生物碱含量平均值约为配方颗粒或合煎的2倍（P<0.01）,吴茱萸次碱单煎含量明显降低（配方颗粒/合煎平均值为单煎的3倍以上,P<0.01）,而吴茱萸碱在配方颗粒与单煎中的差异小（P=0.314）,平均值均在合煎液含量的40%以下（P<0.01）。另外,随着吴茱萸占比提高,合煎液中4种黄连生物碱、吴茱萸碱和吴茱萸次碱含量明显降低,但比例对配方颗粒和单煎影响不大。结论： 在黄连和吴茱萸药对中,黄连生物碱配方颗粒与合煎差异不显著,吴茱萸生物碱在配方颗粒中可能发生转变,导致与合煎有差异,而且配方颗粒并不能重现合煎中药对比例对成分含量的影响趋势。     

提取方式对吴茱萸“质量-毒性”综合评价模式的影响

目的 对不同提取方式提取的吴茱萸中生物碱含量和急性毒性大小进行比较研究,探讨不同提取方式对吴茱萸“含量-毒性”综合评价模式的影响.方法 用HPLC法测定吴茱萸水提组分、醇提组分中吴茱萸碱和吴茱萸次碱的含量,并进行方法学考察;经典急性毒性实验法,进行吴茱萸不同提取物急性毒性比较研究.结果 吴茱萸水提物、醇提物中吴茱萸碱和吴茱萸次碱的百分含量分别为0.028％和0.027％、0.046％和0.075％,水提物组和醇提组无法作出LD50,MTD试验结果按含生药量计算分别为80.0g· kg-1·d-1和70.6g·kg-1·d-1.结论 吴茱萸经不同方式提取后吴茱萸碱和吴茱萸次碱含量和毒性各不相同且各样品均出现死亡,其最大耐受量显示吴茱萸经不同方式的提取均具有毒性,其提取物对小鼠急性毒性强度为:醇提物组＞水提物组;提取物中吴茱萸碱和吴茱萸次碱的含量依次为:醇提物组＞水提物组.说明提取方式对吴茱萸“质量-毒性”综合评价模式有一定的影响,其毒性大小可能与主要化学成分含量存在一定相关性.因此通过“质量-毒性”综合评价模式确定有毒中药的提取方式,更全面、客观、合理.     

参柏克霉泡沫气雾剂质量标准研究

目的建立参柏克霉泡沫气雾剂的质量标准。方法采用薄层色谱（TLC）法对处方中苦参、黄柏、冰片、徐长卿、白花蛇舌草、白鲜皮进行定性鉴别,采用滴定法测定制剂的总生物碱含量。结果TLC法色谱斑点清晰,分离良好,阴性无干扰;制剂的总生物碱含量（以苦参总碱计）不低于0．40mg／mL。结论方法可行、专属性强、重现性好,可作为参柏克霉泡沫气雾剂的质量控制方法。     

Effects of harvesting time and processing on the contents of five alkaloids in the herbaceous stems of Ephedra sinica

In the present study, we studied the changes of the contents of alkaloids in the herbaceous stems of Ephedra sinicaduring different harvest periods as well as before and after processing. The alkaloid contents of 39 batches of ephedra herb, prepared slices ephedra and honey-fried ephedra, 24 batches of ephedra herb with different harvesting periods, which were all collected from cultivation base in Inner Mongolia, and 38 batches of prepared slices ephedra purchased from the market were detected by taking norephedrine (NE), norpseudoephedrine (NPE), ephedrine (E), pseudoephedrine (PE) and methylephedrine (ME) as indicators by using HPLC method. The content of total alkaloid in prepared slices ephedra (1.71%–3.14%) was higher than that in ephedra herb (1.20%–2.53%) and honey-fried ephedra (1.52%–2.99%). Contents of different alkaloids in these three types of samples were significantly different. Prepared slices ephedra and honey-fried ephedra showed significant differences in the contents of NE, NPE and ME (P<0.05), and the contents of E were significantly different between ephedra herb and honey-fried ephedra (P<0.05). The total alkaloid content of ephedra herb was the highest in September (3.10%). Alkaloid contents of prepared slices ephedra collected in the market were uneven and 13%–91% lower than those collected from cultivation base. The results provided a basis for the quality evaluation of ephedra herb and its processed products, and had certain guiding significance for the selection of processed ephedra according to different drug purposes in clinical application. It also provided data support for the harvesting time of ephedra herb.     

The hypotensive and negative chronotropic effects of dehydroevodiamine

The cardiovascular effects of dehydroevodiamine, an alkaloid isolated from Evodia rutaecarpa Jussieu, were studied in both in vivo and in vitro experiments. The in vivo experiments revealed that i.v. administration of dehydroevodiamine elicited a slight but significant reduction in blood pressure and a marked decrease in heart rate which was confirmed by an increased cycle length of the electrocardiogram. However, a hemodynamic experiment with microspheres showed that the total peripheral resistance was not altered by dehydroevodiamine. The blood flows of various organs were not significantly changed except those of kidney and skin, in which blood flow was decreased. In vitro, the spontaneously beating atria were significantly suppressed by dehydroevodiamine in a dose-dependent manner. These findings suggested an important effect of dehydroevodiamine in suppressing the heart, which may largely contribute to the hypotensive effect of this alkaloid. However, its vasodilator effect on hindquarter muscles cannot be neglected.     

Method of Harvesting the Crude Drug Based on Distribution of Alkaloids in the Hook and in the Stem with Hook of Uncaria rhynchophylla1

The distribution of the content of the pharmacologically active oxindole alkaloids in the hook and in the stem of the crude drug "Cho-to-ko" (dried stem with hooks of UNCARIA RHYNCHOPHYLLA) prepared from the cultivated plants were investigated. The total oxindole alkaloid content of the stem was similar to that of the hook portion. It was also found that the area closest to the hook showed a slightly higher alkaloid content than the hook, and that the content of the oxindole alkaloid tended to decrease as the distance from the hook increased. Therefore, the presence of the hook does not affect the quality of the crude drug as far as the oxindole alkaloid content is concerned.     

小果博落回的生药学研究

目的对小果博落回Macleaya microcarpa(Maxim.)Fedde进行显微鉴别和总生物碱含量测定。方法显微鉴别采用形态学和组织学鉴别方法,总生物碱含量测定采用分光光度法。结果小果博落回根、茎、叶薄壁细胞中均含草酸钙结晶;茎、叶的维管束内外均有乳汁管;粉末中可见不定式气孔和非腺毛,导管类型较多。小果博落回总生物碱含量为1.9%～2.7%。结论上述显微特征及总生物碱含量测定可用于小果博落回的药材质量鉴定。