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。     

肺宁合剂提取工艺中甘草和麻黄的配伍规律研究

目的研究肺宁合剂处方中甘草和麻黄的配伍规律。方法以各配伍样品中麻黄碱、伪麻黄碱含量为指标，采用高效液相色谱（HPLC）法测定。结果方中甘草在提取过程中减少了麻黄碱、伪麻黄碱的含量，且麻黄碱的相对减少量多于伪麻黄碱。结论甘草对肺宁合剂中麻黄的有效成分麻黄碱、伪麻黄碱的含量影响明显，反映出了提取过程中甘草麻黄的配伍规律。     

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。     

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) ;…     

十二种国产麻黄的品质评价

本文应用高效液相色谱法对我国24个产地所产的12种麻黄生药进行了六种生物碱的定量分析,这六种生物碱是:麻黄碱(ephedrine),伪麻黄碱(pseudoephedrine),去甲基麻黄碱(norephedrine),去甲基伪麻黄碱(norpseudoephedrine),甲基麻黄碱(methylephedrine)和甲基伪麻黄碱(methylpseudoephedrine)。根据分析结果,对这些麻黄生药的品质作出了评价。     

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。     

麻黄蜜炙前后麻黄碱和伪麻黄碱含量的变化

目的 通过比较蜜炙前后麻黄的主要活性成分麻黄碱和伪麻黄碱的变化,为规范炮制工艺提供科学依据.方法 采用RP-HPLC测定麻黄、蜜炙麻黄中的麻黄碱和伪麻黄碱,使用Kromasil RP-C18色谱柱(250 mm×4.6 mm,5 μm),流动相为0.3%磷酸-甲醇(10:90),检测波长213 nm.结果 6批草麻黄药材经蜜炙后所含麻黄碱及伪麻黄碱,与生品相比分别平均降低0.194%±0.079%和0.153%±0.069%.结论 蜜炙对麻黄中的麻黄碱和伪麻黄碱有明显影响,炮制工艺需规范.     

HPLC测定麻黄及其制剂中3种生物碱含量

目的 建立HPLC同时测定麻黄及其制剂中3种生物碱含量。方法 以乙腈-甲醇-0.1%磷酸溶液(1.5∶4∶94.5)为流动相,同时测定麻黄、金麻杏止咳片和麻杏止咳片中3种生物碱的含量。结果 盐酸麻黄碱、盐酸伪麻黄碱、盐酸甲基麻黄碱的进样量分别为0.102 9~0.686,0.025?11~0.167 4,0.022 23~0.148 2 μg,分别与峰面积呈良好的线性关系;平均回收率分别为100.56%,97.84%和98.42%,RSD分别为0.20%、0.94%和1.31%(n=6)。结论 所建立的HPLC可通过测定3种生物碱的含量综合评价麻黄及其制剂的质量。     

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。     

Simultaneous determination of ephedrine, pseudoephedrine, norephedrine and methylephedrine in Kampo medicines by high-performance liquid chromatography

A simultaneous high-performance liquid chromatographic method for the determination of ephedrine, pseudoephedrine, norephedrine and methylephedrine (ephedrine alkaloids) in Kampo medicines which contain Ephedrae Herba was established. The analysis can be accomplished within 25 min with a Wakosil-II 5C18 HG column by isocratic elution using a mixture of water, acetonitrile and sodium dodecyl sulfate (65:35:0.4) as the mobile phase at a flow-rate of 1.0 ml min(-1), and detection at 210 nm. The detection limits of ephedrine alkaloids are 0.37-1.06 microM per injection (5 microl). This method was applied to analyze the quantities in eight Kampo decoctions; Mao-to, Makyo-yokukan-to, Makyo-kanseki-to, Yokuinin-to, Sho-seiryu-to, Keima-kakuhan-to, Kakkon-to and Kakkon-to-ka-senkyu-sin'i. The concentration (per Ephedrae Herba gram) of ephedrine alkaloids was higher in the Makyo-kanseki-to decoction than in the others. Calcium sulfate from Gypsum Fibrosum raised ephedrine alkaloids dissolution in the Makyo-kanseki-to decoction.     

Simultaneous determination of six alkaloids in ephedrae herba by high performance liquid chromatography

A new and rapid analytical method for the simultaneous determination of six EPHEDRA alkaloids (ephedrine, pseudoephedrine, norephedrine, norpseudoephedrine, methylephedrine, and methylpseudoephedrine) in Ephedrae Herba by high performance liquid chromatography (HPLC) has been developed. Recoveries of each alkaloid were 96.0-101.6% with coefficients of deviation of 1.7-3.0%. The contents of six alkaloids in three species of EPHEDRA indigenous to China are determined and reported.     

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。     

慢支咳喘膏的质量标准研究

目的:建立慢支咳喘膏的质量控制方法。方法:采用薄层色谱(TLC)法对方中麻黄、黄芪、甘草进行鉴别;采用高效液相色谱法对制剂中盐酸麻黄碱和盐酸伪麻黄碱进行含量测定。结果:TLC专属性好、斑点清晰;盐酸麻黄碱、盐酸伪麻黄碱进样量分别在1.3～32.5(r=0.9997)、3.4～85μg(r=0.9998)范围内与其峰面积积分值呈良好线性关系,麻黄碱、盐酸伪麻黄碱的平均回收率分别为97.84%、97.85%,RSD分别为0.63%、1.10%(n均为9)。结论:本试验建立的方法简便、准确、重现性好,能有效控制慢支咳喘膏的质量。     

Determination of ephedra alkaloid and caffeine concentrations in dietary supplements and biological fluids

Dietary supplements containing botanical forms of caffeine and ephedra alkaloids have been widely promoted and used in the U.S. for weight loss and athletic enhancement despite a lack of adequate research on the pharmacology of these botanical stimulants. In order to analyze dietary supplements and perform human pharmacokinetic studies, an analytical approach with good precision and accuracy was needed with sufficient sensitivity to detect very low levels of ephedra alkaloids. A liquid chromatography-atmospheric pressure chemical ionization (APCI) tandem mass spectrometry (LC-MS-MS) method was developed for quantitating the various ephedrine-group alkaloids found in dietary supplements that contain Ephedra species, and in plasma and urine of persons consuming these supplements. Using this method, low nanogram-per-milliliter concentrations of ephedrine, pseudoephedrine, norephedrine, norpseudoephedrine, methylephedrine, methylpseudoephedrine, and caffeine can be quantitated in a 12-min LC-MS-MS run.     

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.     

Ephedra alkaloid contents of Chinese herbal formulae sold in Taiwan

Consumption of Ephedra alkaloids is prohibited in‐competition by the World Anti‐Doping Agency (WADA). In Taiwan, colds are often treated with Chinese herbal formulae containing Herba Ephedrae. We screened products sold in Taiwan and preliminarily assessed their relationships with WADA threshold violations. Fifty‐six concentrated powder products, including 19 Chinese herbal formulae that contained Herba Ephedrae, were collected. The content of Ephedra alkaloids, namely ephedrine (E), methylephedrine (ME), norpseudoephedrine (NPE; cathine), pseudoephedrine (PE), and norephedrine (NE; phenylpropanolamine), was determined using a validated high‐performance liquid chromatography method. The results revealed that the phenotypic indicators of the collected products, E/PE and E/total ratios, were 1.52–4.70 and 0.49–0.72, respectively, indicating that the Herba Ephedrae species in these products was probably E. sinica or E. equisetina, but not E. intermedia. The contents of E, ME, NPE, PE, and NE and the total alkaloid contents in the daily doses of the products were 0.45–34.97, 0.05–4.87, 0.04–3.61, 0.15–12.09, and 0.01–2.00 mg and 0.68–53.64 mg, respectively. The alkaloid contents followed a relatively consistent order (E > PE > ME ≈ NPE > NE), even for products from different manufacturers. We calculated that single doses of 50.0% and 3.6% of the products would result in the WADA thresholds of E and NPE being exceeded, respectively. Our data provide critical information for athletes and medical personnel, who should be wary of using complex Chinese herbal formulae in addition to over‐the‐counter products.