利用高效液相色谱法测定麻黄浸膏中几种麻黄碱的含量

目的:本文采用高效液相色谱法分离测定麻黄浸膏粉中去甲基麻黄碱,去甲基伪麻黄碱,麻黄碱,伪麻黄碱和甲基麻黄碱的含量.方法:最佳流动相组成磷酸二氢钠0.02mol/l(用盐酸和三乙胺调PH至3.2)-甲醇(99.8:0.2).检测波长210nm.流速1.5ml/min.柱温为室温.色谱柱为HIQSIL C18柱.结果:此法重现性较好,各组分均能达到基线分离,工作曲线线性良好.     

HPLC-UV法同时测定麻黄中5种麻黄生物碱的含量

目的建立同时分离检测麻黄中麻黄碱(Ephedrine)、伪麻黄碱(Pseudoephedrine)、去甲麻黄碱(Norephedrine)、去甲伪麻黄碱(Norpseudoephedrine)和甲基麻黄碱(Methylephedrine)的含量测定方法。方法采用HPLC-UV法,色谱柱:苯基柱(Alltima Phenyl,250mm×4.6 mm,5μm);流动相:0.02 mol/L磷酸二氢钾溶液-乙腈(96∶4);流速:0.6 ml/min;检测波长:210 nm;柱温:25℃。结果 5种生物碱在13.5 min内即可达到完全分离,E在2.000 8～40.016 0μg/ml线性关系良好;PE在1.003 6～20.072 0μg/ml线性关系良好;NME在0.199 2～3.984 0μg/ml线性关系良好;NMP在0.200 0～4.00 0μg/ml线性关系良好;ME在0.200 4～4.008 0μg/ml线性关系良好。各生物碱的平均回收率均在92%～104%(RSD≤5.76%)。结论本方法可操作性强,简便快速,分离效果好,重现性好,可为麻黄及含麻黄的中西药制剂提供有效的检测手段。     

麻黄中麻黄生物碱的气相色谱测定法

本文应用毛细管气相色谱法,配备氮磷检测器对麻黄中六种生物碱:麻黄碱、伪麻黄碱、去甲麻黄碱、去甲伪麻黄碱、甲基麻黄碱和甲基伪麻黄碱进行分离、测定。对生药样品预处理方法作了较大改进,采用直接碱化醚提法。简化操作步骤。用内标法,线性方程定最测定了国产十二种麻黄,结果与高效液相色谱法基本一致。     

去甲伪麻黄碱的提取与转化

麻黄中含有十几种生物碱,其中有六种结构相似的生物碱:麻黄碱(一)Ephedrine、伪麻黄碱(+)Pseudo-ephedrine、甲基麻黄碱(-)N-Methylephedrine、甲基伪麻黄碱(+)N-Methylpseudo-ephedrine、去甲麻黄碱(-)Nor-ephedrine、去甲伪麻黄碱(+)Nor-pseudo-ephedrine为人们所熟知。目前国内麻黄碱、伪麻黄碱、甲基麻黄碱已由麻     

尿中麻黄碱类药物的气相色谱检测法

麻黄碱及其类似物有兴奋作用,属体育比赛禁用药。这类化合物的化学结构相似,故有相似的鉴别特征。本文报道了以气相色谱对尿中麻黄碱(ephedrine)、甲基麻黄碱(methylephedrine)、乙基麻黄碱(ethylephedrine)、去甲麻黄碱(norephedrine)及去甲伪麻黄碱(cathine)进行检测,最后以气质联用法进行确证。本法操作简便,灵敏度高,结果可靠。     

木贼麻黄生物碱动态变化的研究

本文用HPLC法研究了宁夏贺兰山和新疆庙几沟地区的木贼麻黄生物碱的动态变化,5种麻黄生物碱为:麻黄碱(E),伪麻黄碱(PE),去甲基麻黄碱(NE),去甲基伪麻黄碱(NPE)和甲基麻黄碱(ME)。在生长期PE居支配地位,文献上流行的论点是E比PE高,而在这些地区的结果则与之相反。总生物碱含量在8月中旬达到高峰,最佳采收期应在初秋,影响含量的主要因素是物候期、降雨量和湿度,对地理位置和气象情况也进行了讨论。     

不同地区市售麻黄药材中盐酸麻黄碱、盐酸伪麻黄碱和总生物碱的含量测定

目的:对全国不同地区市售麻黄药材中盐酸麻黄碱、盐酸伪麻黄碱和总生物碱的含量进行测定,从化学成分的角度对其质量进行评估。方法:收集了28个批次来源于全国7个不同产地、21个不同地区的麻黄药材,按照2010版《中国药典》的方法测定其中盐酸麻黄碱、盐酸伪麻黄碱的含量;建立酸性染料比色法测定药材中的总生物碱。结果:有10个批次的麻黄药材(占全部批次的35.7%)达不到2010版《中国药典》的要求(盐酸麻黄碱和盐酸伪麻黄碱的总质量分数不得少于0.80%),且28个批次的样品中两种生物碱的总质量分数最高与最低相差45倍,总生物碱的质量分数最高与最低相差33倍。结论:所建立的酸性染料比色法测定麻黄总生物碱的含量方法简便、重复性好。市售麻黄药材以草麻黄为主,有效成分生物碱的含量差异较大,劣质情况较为严重。有必要加强麻黄药材的市场监管,保证其临床应用的安全、有效。     

麻黄、含麻黄中成药及生物体液中麻黄碱的定量分析方法

麻黄是一种常用中药 ,为麻黄科多年生草本状小灌木草麻黄 (ＥｐｈｅｄｒａｓｉｎｉｃａＳｔａｐｆ.)或木贼麻黄(Ｅ .ｅｑｕｉｓｅｔｉｎａＢｕｎｇｅ .)和中麻黄 (Ｅ .ｉｎｔｅｒｍｅｄｉａＳｃｈｒｅｎｋｅｔＭｅｙ .)的草质茎 ,是提取麻黄碱和制成多种制剂的原料。麻黄含生物碱 10种以上 ,主要是 3对立体异构的生物碱 ,即 :左旋麻黄碱 (ｌ -ｅｐｈｅｄｒｉｎｅ) ,右旋伪麻黄碱 (ｄ -ｐｓｅｕｄｏｅｐｈｅｄｒｉｎｅ) ;左旋去甲基麻黄碱 (ｌ-ｎｏｒｅｐｈｅｄｒｉｎｅ) ,右旋去甲基伪麻黄碱 (ｄ -ｎｏｒｐｓｅｕｄｏｅｐｈｅｄｒｉｎｅ) ;…     

麻黄-桂枝配伍对麻黄类生物碱、桂皮酸及桂皮醇在大鼠体内药动学的影响

目的建立UPLC-MS/MS法,对麻黄-桂枝药对提取物、单味麻黄提取物和单味桂枝提取物中麻黄类生物碱、桂皮醇及桂皮酸的血浆药动学进行比较研究,探讨中药复方配伍对药效成分体内过程的影响。方法实验大鼠分别灌胃麻黄、桂枝及麻黄-桂枝提取物,测定不同时间点大鼠血浆中麻黄类生物碱、桂皮醇和桂皮酸的浓度,采用DAS3.0软件计算药动学参数,SPSS13.0对两组的药动学参数进行统计分析。结果麻黄-桂枝组中去甲基麻黄碱、去甲基伪麻黄碱、麻黄碱、伪麻黄碱和甲基麻黄碱的达峰浓度(C_(max))均明显大于麻黄组(P<0.05);麻黄-桂枝组中去甲基伪麻黄碱的药时曲线下面积(AUC_(0-t))明显大于麻黄组(P<0.05);麻黄-桂枝组中去甲基麻黄碱、麻黄碱、伪麻黄碱和甲基麻黄碱的平均驻留时间(MRT_(0-t))均明显小于麻黄组(P<0.05);麻黄-桂枝组中去甲基麻黄碱、麻黄碱和甲基麻黄碱的半衰期(T_(1/2z))明显小于麻黄组(P<0.05)。麻黄-桂枝组中桂皮醇、桂皮酸的AUC_(0-t)和MRT_(0-t)均明显大于桂枝组(P<0.05)。结论麻黄与桂枝配伍后,增加了5种麻黄生物碱在体内的吸收浓度,延缓了去甲麻黄碱、麻黄碱、伪麻黄碱和甲基麻黄碱在体内的消除,提高了桂皮醇和桂皮酸的生物利用度。     

麻黄挥发油对麻黄碱和伪麻黄碱经Caco-2细胞转运特征的影响

摘要：目的:基于"性味药理"研究思路,选取麻黄挥发油和生物碱作为其辛温解表主要功效成分,从药物吸收转运角度研究麻黄解表发散的作用原理。方法:采用Caco-2细胞转运模型,HPLC同步对比分析麻黄挥发油加入对麻黄碱和伪麻黄碱从板顶端（AP）→底端（BL）及BL→AP的双向转运过程的影响,计算表观渗透系数,并分析挥发油对其转运特征的影响。结果:麻黄碱和伪麻黄碱的Caco-2细胞表观渗透系数(Papp)与浓度无显著关系。麻黄碱的Papp（AP→BL）约为19×10-6cm·s-1,伪麻黄碱的Papp（AP→BL）约为16×10-6cm·s-1,吸收作用均较好,外排率均值为0.72,推测其转运过程主要为被动转运过程。麻黄挥发油促进麻黄碱和伪麻黄碱的转运吸收,其对伪麻黄碱促进吸收作用更为显著。结论:挥发油和生物碱在麻黄解表发散功效可能存在协同作用。     

Survey on resources of Ephedra plants in Xinjiang

The resources of wild Ephedra plants in the Xinjiang Uygur Autonomous Region were surveyed. Ephedra plants mainly grow on the fringes of the Taklimakan Desert and Gureban-tonggute Desert. We found six genotypes of Ephedra przewalskii growing widely in Xinjiang. Three genotypes of Ephedra intermedia were limited to the northern and eastern parts, and Ephedra regeliana scattered in the northern part of Xinjiang. These Ephedra specimens were analyzed for DNA sequences of nuclear ribosomal DNA, internal transcribed spacers 1 and 2, chloroplastic DNA, trnL intron and trnL-trnF intergenic spacer. Intraspecific variation of the nucleotide sequence in E. przewalskii was found in different habitats. Norephedrine, ephedrine, pseudoephedrine, and methylephedrine contents of the specimens were determined. Although Ephedra intermedia of all three genotypes contained ephedrine alkaloids, ephedrine alkaloids were not detected in E. regeliana and E. przewalskii.     

Studies on cultivated ephedra plants in inner mongolia autonomous region and ningxia hui autonomous region

Progression of the desertification in northern China has been causing damage to wild Ephedra plants on which we depend for most of supply of the traditional herbal medicine, "Ma huang." The Chinese government encourages the cultivation of Ephedra plants, and Ephedra fields have been reclaimed in the original Ephedra habitats in recent years. We surveyed 7 Ephedra fields that have been recently developed in the Inner Mongolia Autonomous Region and Ningxia Hui Autonomous Region to collect information on Ephedra plant cultivation, especially pertaining to crop species. Specimens taken from those Ephedra fields were genetically and morphologically analyzed, and their ephedrine alkaloid content was examined. DNA analyses of Ephedra specimens, including DNA sequencing of ITS (internal transcribing sequence of nuclear ribosomal DNA) and trn L/F (intron of trnL and intergenic spacer between the trnL and trnF of chloroplast DNA) region and species-specific amplification of trn L/F were conducted to identify Ephedra species. Based on the results of DNA sequencing and morphological determination, the crops grown in 6 fields ware identified as Ephedra sinica, while co-planting of E. sinica and E. intermedia was found in one field where a higher appearance rate of plants with varied morphology from wild Ephedra plants was observed. Furthermore, direct sequencing of the PCR product of the trn L/F region of some specimens from the field and their species-specific PCR showed ambivalent result. Cloning and sequencing of the PCR product of the trn L/F region of those specimens DNA suggested their heteroplasmy, containing both E. sinica- and E. intermedia-type chloroplasts. On the other hand, the profile of the ephedrine alkaloid content was clearly correlated with the result of direct sequencing of the trn L/F region; the specimens showing the E. sinica-type sequence contained more ephedrine than pseudoephedrine, and the specimens of the E. intermedia-type more pseudoephedrine.     

内蒙西部草麻黄中生物碱的动态研究

本文应用高效液相色谱法研究了内蒙西部草麻黄主产区麻黄生物碱的动态变化。样品均采自该区两个固定观测区(5M~2以内),数量多,目前已成为定期供应工厂提取地区。在一般年份,生长期间麻黄碱与伪麻黄碱之比几乎平行,其总生物碱的含量在7月和10月初达高蜂,较之其它地区高(约2.5％)。     

A comparative study of commercial samples of ephedrae herba

A total of 22 commercial Ephedra herba samples which belonged to EPHEDRA SINICA, E. INTERMEDIA, E. EQUISETINA, and E. DISTACHYA, respectively, were collected from the Taiwan herbal market. The contents of the six ephedrine alkaloids - ephedrine (E), pseudoephedrine (PE), methylephedrine (ME), methyl-pseudoephedrine (MPE), norephedrine (NE), and nor-pseudoephedrine (NPE) - in these samples were determined by capillary electrophoresis and were found to differ greatly among the samples. Generally, E. SINICA was superior (1.594 +/- 0.467%) and E. INTERMEDIA was inferior (1.210 +/- 0.372%). Among the individual constituents, the sum of E and PE contents in each sample was about nine-tenths of the total alkaloids, and the ratios of E/PE, ME/MPE, and NE/NPE in the given species were definite and could be used to aid in identifying the origin of the herbs. The alkaloid contents were found to be higher in the internodes of the herbs and in those items with thin stems, more powdery and less fibrous characters. There were no indications for alkaloids in the roots of the plants.     

近红外漫反射光谱法结合CP-ANN和PLS高通量分析草麻黄药材

目的:建立草麻黄药材的近红外漫反射光谱高通量分析方法。方法:测量草麻黄样品的近红外漫反射光谱(near infra-red diffuse reflectance spectra,NIRDRS),应用化学计量学技术进行光谱处理和数据预处理,分别建立并验证草麻黄药材的产地和采摘时间判别对向传播人工神经网络(counter-propagation artificial neural network,CP-ANN)模型及麻黄碱和伪麻黄碱含量预测偏最小二乘(partial least square,PLS)模型。结果:草麻黄药材的产地和采摘时间判别CP-ANN模型的验证样品预测准确率分别为100.0%和80.0%;麻黄碱和伪麻黄碱含量预测PLS模型的验证样品预测均方根误差(root mean square errors ofprediction,RMSEPs)小,分别为1.12和0.236,预测值与参考值的相关系数(correlation coefficients)大,分别为0.9721和0.9309。结论:采用所建方法能同时对草麻黄药材的产地和采摘时间进行准确判别,对其麻黄碱和伪麻黄碱的含量进行准确预测。该方法准确、快速,无需特殊的样品处理,也不使用化学试剂。     

必克敏胶囊质量标准的研究

目的 :控制必克敏胶囊的质量。方法 :采用薄层层析法对处方中的麻黄进行定性研究 ,对成品乌头碱限量进行了检查 ;采用高效液相色谱法测定了必克敏胶囊中麻黄碱和伪麻黄碱的含量。结果 :麻黄碱和伪麻黄碱的标准曲线分别在0.02～0.10mg/ml(r=0.9993)和0.01～0.05mg/ml(r=0.9996)之间有较好的线性关系 ,麻黄碱和伪麻黄碱的加样回收率分别为 (101.4±1.78) %和(98.08±1.81) %。结论 :鉴别方法专属性强 ,定量方法灵敏 ,可有效地控制必克敏胶囊的质量     

Concentrations of ephedra alkaloids and caffeine in commercial dietary supplements

Dietary supplements that contain Ma Huang (ephedra alkaloids) and guarana (caffeine) are widely marketed and used in the U.S. for weight loss and athletic performance enhancement, despite a lack of adequate research on the pharmacology of these botanical stimulants. We developed and applied a novel liquid chromatography-tandem mass spectrometry (LC-MS-MS) method to quantitate the various ephedra alkaloids found in dietary supplements that contain Ephedra species. The quantities of ephedrine, pseudoephedrine, norephedrine, norpseudoephedrine, methylephedine, methylpseudoephedrine, and caffeine were determined for 35 commercial dietary supplements and compared with the amounts listed on the product labels. The total ephedra alkaloid content ranged from 5.97 mg to 29.3 mg per serving. Two supplement brands did not list the quantity of ephedra alkaloids on the label, and four did not list the amount of caffeine per serving. Of the products tested, 31% contained > 110% of the total ephedra alkaloids listed on the label, and 6% of the supplements contained < 90% of the listed amount. For caffeine, 86% of the product lots that listed the caffeine amount contained less than 90% of the labeled quantity. No products contained > 110% of the declared caffeine content. The total ephedra alkaloid content varied significantly from lot to lot in 5 of 9 products. Three product brands contained proportions of alkaloids that exceeded amounts reported for E. sinica, including one that was 98% ephedrine, one that had 10% norpseudoephedrine, and one that contained an average of 13% methylephedrine. We conclude that product inconsistency is common among some commercially available dietary supplements that contain ephedra alkaloids and caffeine.     

国产麻黄的形态组织学研究——Ⅱ.西南主产种及其它种

本文报道我国西南产麻黄——丽江麻黄Ephedra likiangensis Florin、匍枝丽江麻黄E.likiangensis f.mairei(Florin)C.Y.Cheng、藏麻黄E.saxatilis Royle ex Florin、山岭麻黄E.gerardiana Wall、垫状山岭麻黄E.gerardiana Var.congesta C.Y.Cheng、矮麻黄E.minuta Florin和异株矮麻黄E.minuta var.dioeca C.Y.Cheng,以及形态组织特征较特殊的宁夏产斑子麻黄E.lepidosperma C.Y.Cheng、新疆产窄膜麻黄E.lomatolepis Schrenk,西藏产西藏中麻黄E.intermedia var.tibetica Stapf的生药形态组织学研究结果。并根据对国产麻黄的生药形态组织学的系统研究结果,分别编写了各种国产麻黄(包括13种3变种1变型)的生药性状和生药显微特征检索表。