TLC—HPLC法测定小活络丸内中乌头碱,次乌头碱和乌头碱的含量

采用ＴＬＣ－ＨＰＬＣ法测定小活络丸内中乌头碱、次乌头碱和乌头碱的含量，在硅胶Ｇ薄层板上以石油醚－正己烷－醋酸乙酯－无水乙醇－浓氨水（１：２：５：５：０．５）为展开剂，分离提取酯型三，用Ｒｅｓｏｌｖｅ Ｓｐｈｅｒｉｃａｌ Ｓｉｌｉｃａ柱，以无水乙醇－０．４％醋酸铵水溶液（９７：３）为流动相进行测定，检测波长２３１ｎｍ，平均回收率：８３．２％（中乌头碱）、９２．１（次乌头碱）、８４．１％（乌头碱）。     

LC-MS法同时测定雷公藤浸膏中雷公藤新碱和雷公藤碱戊含量

目的建立一种灵敏、准确的雷公藤浸膏中雷公藤新碱和雷公藤碱戊含量的LC-MS法。方法雷公藤浸膏样品经氯仿溶解后用稀盐酸（2．0mol·L“）溶液提取,上清液移人Oasis。MCX固相萃取小柱进行净化,然后样品在ZorbaxPlusRRHDC18柱（50innl×2．1mm,1．8μm）上,以醋酸铵缓冲液[0．05％醋酸一酸酸铵溶液（5mmol·L-1）]-乙腈（30：70）为流动相进行分离,应用LC—MS法,在大气压化学电离正离子选择离子监测模式（SIM）下测定,雷公藤新碱和雷公藤碱戊的定量离子分别为m／z806和m／z779。结果雷公藤新碱和雷公藤碱戊的绝对回收率为87．0％-97．5％,在含量1．0—200．0μg·kg-1内均具有良好线性,日内RSD均〈9．8％,日间RSD均〈14．7％,定量检出限均为1．0μg·kg-1。结论本方法简便、灵敏、干扰少、特异性好,可用于雷公藤浸膏中雷公藤新碱和雷公藤碱戊含量的监测。     

中药祁州漏芦中的新植物甾酮

祁州漏芦为菊科漏芦属祁州漏芦〔Ｒｈａｐｏｎｔｉｃｕｍｕｎｉｆｌｏｒｕｍ（Ｌ．）ＤＣ．〕的干燥根．具有清热解毒、舒筋通络的功效．利用大孔树脂、硅胶柱层析及ＨＰＬＣ反相柱色谱法从中分离得到两个新的植物甾酮类成分，其中一个命名为漏芦甾酮Ｒ１（ｒｈａｐｏｎｔ...     

TLC一HPLC法测定小活络丸内中乌头碱、次乌头碱和乌头碱的含量

采用ＴＬＣ－ＨＰＬＣ法测定小活络丸内中乌头碱、次乌头碱和乌头碱的含量。在硅胶Ｇ薄层板上以石油醚（６０～９０℃）－正己烷－醋酸乙酯－无水乙醇－浓氨水（１：２：５：５：０．５）为展开剂，分离提取酯型生物碱，用Ｒｅｓｏｌｖｅ　Ｓｐｈｅｒｉｃａｌ　Ｓｉｌｉｃａ柱（５μｍ，１５０ｍｍ×３．９ｍｍ），以无水乙醇－０．４％醋酸铵水溶液（９７：３）为流动相进行测定，检测波长２３１ｎｍ，平均回收率：８３．２％（中乌头碱）、９２．１（次乌头碱）、８４．１％（乌头碱）。     

雷公藤明碱、异雷公藤春碱及异雷公藤内酯四醇的免疫抑制作用

雷公藤明碱（简称明碱）、异雷公藤春碱（简称异春碱）、异雷公藤内酯四醇（简称异四醇）是从福建泰宁县产雷公藤根皮中经化学法提取的新单体〔１,２,３〕。本文研究它们的免疫抑制作用。１材料１１动物ＩＣＲ和Ｃ５７ＢＬ小鼠,（２０±２）ｇ,购自上海ＢＫ实验动物...     

雷公藤化学成分研究

摘 要 目的：研究雷公藤根的化学成分。方法: 通过硅胶柱色谱、Sephadex LH 20凝胶色谱和制备高效液相色谱等方法进行化合物分离纯化,根据理化性质和波谱数据确定其结构。结果: 从雷公藤根中分离鉴定了12个化合物,分别为：雷公藤吉碱（1）、雷公藤次碱（2）、雷酚萜甲醚（3）、任卡漆 5 烯 3β,28 二醇（4）、雷酚萜E（5）、雷酚萜L（6）、maytenoic acid（7）、雷酚内酯（8）、雷公藤红素（9）、去甲泽拉木醛（10）、1 desacetyl wilforgine（11）、雷公藤春碱（12）。结论: 首次对化合物1和2的1D、2D核磁数据进行全归属,并运用X ray单晶衍射技术确定了化合物1 的绝对构型。     

HPLC法测定马钱子及其制剂中士的宁与马钱子碱的含量

报道了采用ＨＰＬＣ法测定马钱子及其制剂中士的宁与马钱子碱的含量。色谱填料为硅胶，流动相为正己烷－二氯甲烷－甲醇－浓氨试液（４７．５：４７．５：０．３５），检测波长为２５４ｎｍ。实验结果表明，该方法简便，准确，灵敏度高，重现性好。     

HPLC法测定雷公藤粗制品中雷公藤甲素的含量

目的：建立高效液相色谱法测定雷公藤粗制品中雷公藤甲素的含量。方法：雷公藤粗制品经洗脱提取后，采用十八烷基键合硅胶柱，以乙腈-水（30：70）为流动相，以218nm为检测波长，检测雷公藤粗制品中雷公藤甲素的含量。结果：雷公藤甲素在1．92～11．52μg／ml范围内线性良好，r=0．9999，平均回收率为95．32％，RSD为1．16％。结论：本法操作简便、结果准确，可用于雷公藤粗制品中雷公藤甲素的含量测定。     

紫杉醇提取纯化工艺

以云南红豆杉树皮（或树叶）为原料，提取纯化紫杉醇。先经９５％乙醇、二氯甲烷提取，再经硅藻土柱涂渍色谱、硅胶６０中压快速柱色谱分离，收集含紫杉醇－ｃｅｐｈａｌｏｍａｎｎｉｎｅ的组分后以Ｃ_（１８）制备型ＲＰ－ＨＰＬＣ分离，两次结晶后得到紫杉醇无色结晶固体，纯度≥９８．８％，收率为树皮干重的０．０２８％，树叶干重的０．００８８％。     

反相离子对HPLC法测定天仙子中的生物碱及TLC法鉴别天仙子和南天仙子

本文用离子对ＨＰＬＣ法测定了天仙子中莨菪碱和东莨菪碱的含量。莨菪碱和东莨菪碱的样品量与峰面积积分值的线性范围分别为０．２４４５～０．７３３２μｇ，ｒ＝０．９９９５和０．１８６４～０．５５９２μｇ，ｒ＝０．９９９９；平均回收率分别为：９８．８２％，ＲＳＤ＝３．４１％（ｎ＝５）和９７．８６％，ＲＳＤ＝１．８５％（ｎ＝５）。样品被处理后，所得色谱图分离度好，无干扰。并用ＴＬＣ法对天仙子（含中亚天仙子）和南天仙子进行了鉴别。为评价天仙子的真伪优劣提供了科学依据。     

Chemical constituents and analgesic activity of Aconitum kusnezoffii Reichb.

In the present study,we aimed to investigate the chemical constituents and analgesic activity of Aconitum kusnezoffii Reichb. The isolation and purification of components were achieved by a series of chromatography, including silica gel, Sephadex LH-20 and HPLC. By using spectroscopic analysis, their structures were identified. Using PDE-4A as analgesic target, moleculardocking was conducted between isolated compounds by using Schrodinger software. Neoline is a typical non-ester diterpene alkaloid. It was studied by using the mouse torsion body method and hot plate method. A total of 12 diterpene alkaloids were obtainedand identified as Mesaconitine(1), Bewutine (2), Bewudine (3), Songoramine (4), Songorine (5), Neoline (6), Talasamine (7), isotalatizidine (8), Hokbusine A (9), Mesaconine (10), 8-OEt-14-benzoylmesaconine (11), 8-Methoxy-14-benzoyl-beiwutinine (12).Compounds 9 and 12 were isolated from Aconitum kusnezoffii Reichb. for the first time. Twelve diterpenealkaloids could act on the analgesic target. Neoline is a typical non-ester diterpene alkaloid. It had significant analgesic effect. Diterpene alkaloids were the main components of Aconitum kusnezoffiiReichb., and they had good analgesic activity.     

大理藜芦碱B的结构及其绝对构型的确定

从云南产的大理藜芦(Veratrum taliense)的全草中分离得一个维藜芦碱类的新生物碱,命名为大理藜芦碱B(vertaline B,I)除了应用光谱分析测定其结构外,并对I的氢溴酸盐单晶进行了X-ray衍射分析,确定了I的绝对构型为(20R,22R,25S)22,26-缩亚胺胆甾烷-5-烯-3β,16β,20β-三醇[(20R,22R,25S)22,26-epiminocholest-5-ene-3β,16β,20β-triol]。此外,尚分离得二个已知甾体生物碱,介藜芦胺(jervine,Ⅱ)和狭叶藜芦碱乙(stenophlline B,Ⅲ)。     

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。     

中药色谱及光谱分析方法研究 二 山豆根总碱及注射剂的薄层分析及HPLC制备

山豆根总碱及其注射剂用 CHCl_3-EtOH-NH_3·H_2O(80:15:5)为展开剂,薄层径向展开可获得15～18个斑点、其中7～8个斑点为生物碱。用 HPLC 制备,以普通硅胶为柱填料,可分离出8个馏分。主要馏分用红外 ATR 法证明为山豆根碱(Dauricine)及去甲山豆根碱(Dauricinoline)。方法简便、快速。     

Detection of sulphur-conjugated pyrrolic metabolites in blood and fresh or fixed liver tissue from rats given a variety of toxic pyrrolizidine alkaloids.

Rats were given single injections of hepatotoxic pyrrolizidine alkaloids and killed after 30 h. Sulphur-bound pyrrolic metabolites from the alkaloids in samples of their blood or liver tissue were converted to extractable ethyl ethers of low molecular weight for detection and identification using TLC, HPLC or GC-MS. Liver samples were also preserved as an acetone-washed powder or in formalin-based fixative before being later subjected to similar analyses. S-Bound pyrrolic metabolites were identified in samples from rats given all the types of alkaloid tested, which included mono-esters (heliotrine, indicine), a diester (lasiocarpine), and macrocyclic diesters (retrorsine, senecionine). The pattern of pyrrolic metabolites from the crotanecine-based alkaloid anacrotine differed and could be distinguished from retronecine- or heliotridine-based alkaloids. Whereas the alkaloids tested ranged widely in toxicity, single doses of 0.25 x acute LD50 or more led to detectable metabolites. Liver pyrroles remained detectable in fixed or powdered samples preserved for long periods. Similar tests on rats given monocrotaline continuously in their drinking water (20 mg/l) led to detectable pyrroles in blood after 12 days (total intake approx. 27 mg/kg) and in liver after 25 days. The metabolites remained detectable in rats killed 17 days after the alkaloid exposure was discontinued. The simple procedures described are applicable to the diagnosis of pyrrolizidine alkaloid exposure in livestock, using fresh or dried blood or fresh or preserved liver samples. They bring to pyrrolizidine toxicology for the first time the capability to demonstrate chemically that livestock (or people) have been exposed to these alkaloids many days or weeks previously.     

黄连中生物碱有效部位纯化工艺研究

目的：用大孔吸附树脂对黄连总生物碱有效部位进行纯化工艺研究。方法：以总生物碱吸附量、含量和解吸率为考察指标,采用高效液相色谱法检测黄连中总生物碱的含量。结果：HPD722型大孔吸附树脂对黄连总生物碱有良好吸附分离性能,适宜的工艺条件为：黄连药材上样液质量浓度为100mg·ml^-1（相当于原生药）,上样体积为3BV湿树脂体积,洗脱方法为先以5BV湿树脂体积蒸馏水除去杂质,再以7BV湿树脂体积50％乙醇洗脱,收集50％乙醇洗脱部分。结论：该法简单可行,适合工业生产。     

川乌不同煎煮时间总生物碱与酯型生物碱含量变化趋势对比

目的:以川乌为研究对象,比较其在不同煎煮时间的煎剂中总生物碱、酯型生物碱类成分的变化趋势。方法:采用滴定法及高效液相色谱法,对川乌在不同煎煮时间煎剂中的总生物碱及酯型生物碱进行测定。并以此为指标,考察其在不同煎煮时间的煎剂中有效成分及主要毒性成分变化趋势。结果:在煎煮0～4h的川乌煎剂中,随煎煮时间延长,其有效成分总生物碱含量呈现上升趋势,而主要毒性成分则呈现下降趋势。结论:为了使毒性药物川乌的使用符合"低毒高效",完善药典相关内容,应进一步明确双酯型生物碱与单酯型苯甲酰类乌头碱在川乌及其制剂中的含量及二者的比例。     

Plant antitumor agents. 22. Isolation of 11-hydroxycamptothecin from Camptotheca acuminata Decne: total synthesis and biological activity

The antitumor alkaloid 11-hydroxy-(20S)-camptothecin was isolated from the woody tissue of Camptotheca acuminata. Structural proof derived from comparison with racemic 4 prepared by total synthesis. Antitumor activity of racemic 4 in L1210 leukemia in mice was considerably greater than that of natural (20S)-camptothecin and its sodium salt. There was also no toxic effect observed even at relatively high doses.     

应用紫外分光光度法测定苦参总碱的含量

用岛津UV-210紫外分光光度计对苦参膏中苦参总硷的含量进行了测定。结果表明，苦参总硷的光谱图在200nm处有最大吸收，并且吸收值与苦参总硷的含量间存在着良好的线性关系。并对苦参总硷在水溶液中的稳定性和实验方法的精密度进行了考察，认为此方法适合于作含量测试分析，其平均回收率为103.2%。     

Content versus label claims in ephedra-containing dietary supplements.

The content of ephedra alkaloids in herbal dietary supplements containing ephedra (ma huang) was studied. The ephedra alkaloid content of 20 ephedra-containing supplements was determined by high-performance liquid chromatography. Contents of (-)-ephedrine, (+)-pseudoephedrine, (-)-methylephedrine, (-)-norephedrine, and (+)-norpseudoephedrine were measured. Ephedra alkaloid content varied considerably among products. Total alkaloid content ranged from 0.0 to 18.5 mg per dosage unit. Ranges for (-)-ephedrine and (+)-pseudoephedrine were 1.1-15.3 mg and 0.2-9.5 mg, respectively. (+)-Norpseudoephedrine, a Schedule IV controlled substance, was often present. Significant lot-to-lot variations in alkaloid content were observed for four products. For one product, lot-to-lot variations in the content of (-)-ephedrine, (+)-pseudoephedrine, and (-)-methylephedrine exceeded 180%, 250%, and 1000%, respectively. Half of the products exhibited discrepancies between the label claim for ephedra alkaloid content and actual alkaloid content in excess of 20%. One product was devoid of ephedra alkaloids. Assay of 20 ephedra-containing dietary supplements showed that alkaloid content often differed markedly from label claims and was inconsistent between two lots of some products.