大黄中芦荟大黄素等5种蒽醌成分含量测定方法的探索研究

目的:为大黄中游离蒽醌的含量测定探索更加适宜的检测条件.方法:通过对在254 nm和440 nm检测波长处获得的5种指标性蒽醌类成分图谱形状、分离程度的分析,对比此两个波长处检出结果的优劣.结果:在440 nm处芦荟大黄素和大黄酸受干扰最小,图谱基线平稳,干扰峰较少,分离效果理想.结论:大黄中游离蒽醌含量测定在440 ...     

气象因子对唐古特大黄蒽醌类成分含量的影响分析

目的:研究气象因子对青海唐古特大黄蒽醌类成分含量的影响。方法:采用高效液相色谱法测定不同生境的唐古特大黄中蒽醌类成分的含量,通过偏相关分析研究气象因子对唐古特大黄蒽醌类成分含量的影响。结果:不同生境的唐古特大黄中蒽醌类成分含量有较大差异。偏相关分析结果表明,温度对大黄酚和大黄素甲醚含量的影响较为显著,而降水和日照对蒽醌类成分含量无明显影响。结论:温度是影响唐古特大黄蒽醌类成分含量的主要气象生态因子。     

5个蒽醌三三配伍治疗脑缺血大鼠的药代动力学研究

目的:建立LC-MS方法测定大鼠血浆中蒽醌成分含量,探讨5个大黄蒽醌成分(芦荟大黄素、大黄素、大黄酸、大黄酚、大黄素甲醚)三三配伍时在脑缺血大鼠模型中的药代动力学特征.方法:MCAO法制备大鼠局灶性脑缺血模型.模型大鼠随机分成11组,空白组1组,给药组10组.给药组将5个大黄蒽醌三三结合,给药剂量:芦荟大黄素(A) 1...     

基于叶绿体基因matK及UPLC对市售大黄的种质资源鉴定和质量分析

大黄是多基原大宗常用药材,不同基原大黄其药理活性存在一定差异。本研究基于叶绿体基因matK序列对市售大黄饮片的种质资源进行鉴定,通过UPLC对其总蒽醌和游离蒽醌含量进行测定,以期确定市售大黄的主要种质及质量。本研究从27省40市收集89份市售大黄样品并提取DNA,通过PCR扩增matK基因,扩增的matK基因序列的分析结果表明,收集的市售大黄样品都是同一基原,即掌叶大黄,共鉴定了其8个基因型:Rp1、Rp2、Rp3、Rp4、Rp5、Rp6、Rp10和Rp12,其中来自甘肃、四川和云南省的Rp4和Rp6是主要流通基因型,分别占总样品量40.45%和37.08%。系统发育树结果表明, 8个基因型主要分成2大支,其中主要基因型Rp4和Rp6聚在同一大支,遗传距离分析结果表明8个基因型遗传距离在0.001～0.010之间。利用UPLC检测市场样品中的总蒽醌和游离蒽醌含量结果表明, 93.26%样品符合药典标准。样品之间总蒽醌含量和游离蒽醌的含量差异显著,其中游离蒽醌相差1.01%;总蒽醌含量相差3.79%,说明市售大黄样品质量存在参差不齐的现象,但是不同采集省份之间市售大黄总蒽醌和游离蒽醌含量...     

不同炮制方法大黄饮片在贮存过程中蒽醌成分的含量变化分析

目的分析不同大黄炮制方法对饮片贮藏过程中蒽醌类成分含量变化的影响.方法 对3种大黄饮片1～12个月贮藏样品采用超高效液相色谱仪,检测其中的大黄酸、芦荟大黄素、大黄酚、大黄素和大黄素甲醚的含量变化.结果 5种蒽醌类成分在贮存过程中都存在明显下降的趋势,大黄酚及大黄素甲醚的含量下降尤为明显.不同饮片中,熟大黄中的蒽醌类成分含量变化较小,酒大黄中蒽醌类成分的含量下降明显.结论 不同炮制方法对大黄饮片贮藏过程中的蒽醌类成分的含量变化影响不同,虽然随贮藏时间的增加蒽醌类成分含量均有所下降,但以熟大黄变化最小,酒大黄变化最为明显.     

比色法测定巴天酸模水提物中蒽醌类成分的含量

目的 测定巴天酸模水提取物中蒽醌类成分的含量.方法 运用比色法,以1,8-二羟基蒽醌为对照品,用0.8％乙酸镁甲醇溶液显色;在510 nm波长处测定巴天酸模水提取物中蒽醌类成分含量.结果 巴天酸模水提取物中蒽醌类成分含量达到31.07 mg/g,以结合型蒽醌为主.结论 比色法简便、精确、重现性好,可以作为巴天酸模水提取物中蒽醌类成分的含量测定方法.     

清肠饮中大黄蒽醌含量的比色分析方法研究

目的:建立一种测定清肠饮中大黄蒽醌含量的比色分析方法.方法:采用5%氢氧化钠 2%氢氧化铵混合碱液和0.5%醋酸镁 甲醇液两种比色法对样品的含量进行比较研究.结果:醋酸镁 甲醇比色法灵敏、简便、准确且稳定性好.结论:醋酸镁 甲醇比色法可作为测定大黄中蒽醌类含量的常规分析方法.     

决明子发酵前后5种蒽醌类成分变化研究

目的:探讨固态发酵对决明子中5种蒽醌类成分含量的影响。方法:采用高效液相色谱法测定决明子发酵前后芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的含量并进行对比研究。色谱柱为C18-ODS反相柱(250mm×4.6mm,5μm),流动相为甲醇-0.1%磷酸水溶液(梯度洗脱),流速为1mL.min-1,检测波长为280nm。结果:决明子经过发酵后,游离型蒽醌含量呈上升趋势。以未发酵成分含量为100%计算,5种成分变化分别为104.6%、102.2%、93.4%、215.6%、134.8%,其中芦荟大黄素、大黄酸和大黄素变化不明显,大黄酚与大黄素甲醚分别增加至2.15倍和1.34倍,可见发酵增加了蒽醌苷元的含量。结论:决明子通过发酵,有利于增加活性成分蒽醌苷元的含量。     

大孔吸附树脂法纯化大黄中结合型蒽醌总提取物的研究

大黄为常用中药，主要成分为蒽醌类、二苯乙烯苷类、色酮类及鞣质等化合物。结合型蒽醌类成分水溶性大。通常认为是利胆和泻下的主要成分，而大黄酚、大黄素、大黄素甲醚等游离蒽醌苷元几乎无泻下活性。传统提取工艺复杂，且提取物杂质含量较高，特别是制备注射剂时蒽醌苷元及鞣质类成分常常对溶液的澄明度产生较大的影响。我们以大孔吸附树脂柱色谱法分离大黄中结合型蒽醌提取物，采用比色法考察总提取物中结合型蒽醌的含量．为大黄提取物的纯化与精制生产工艺作一新的尝试。     

新疆3种独尾草总蒽醌和芦荟大黄素含量的比较

目的:比较新疆3种独尾草在开花期和休眠期总蒽醌的含量以及根、茎、叶中芦荟大黄素的含量。方法:用超声波法提取独尾草中的总蒽醌,采用紫外分光光度法测定总蒽醌的含量,用HPLC法测定3种独尾草根、茎、叶中芦荟大黄素的含量。结果:总蒽醌含量,异翅独尾草根中最高,且在休眠期高于开花期;芦荟大黄素含量,根>叶>茎;异翅独尾草根中含量最高,粗柄独尾草茎中最低。结论:新疆3种特有独尾草中,异翅独尾草在休眠状态时根中贮藏的总蒽醌和芦荟大黄素含量最高。     

不同配比何首乌、牛膝药对指纹共有模式和基于主成分分析的等级评价研究

目的:通过比较有效成分含量及共有峰的主成分,对不同配比何首乌牛膝药对的等级进行评价。方法:采用RP-HPLC梯度洗脱法同时测定10个不同比例何首乌牛膝药对中4种成分含量,同时标定共有峰,采用SPSS进行聚类分析和主成分分析。结果:有效成分含量测定结果显示,何首乌牛膝药对1∶1、2∶1、4∶3、5∶2比例较好。何首乌、5∶2药对可聚为一类,1∶1和3∶2药对可聚为一类,3∶4与4∶3药对可聚为一类。主成分分析显示何首乌牛膝药对2∶1、4∶3、1∶1评分较高。结论:不同配比药对对有效成分溶出影响较大,从有效成分角度考虑1∶1、2∶1和4∶3比例何首乌牛膝药对评分较高。     

Clinical analysis of liver injury caused by Chinese patent medicines containing Polygonum multiflorum

In the present study, we discussed the drug-induced liver injury caused by Chinese patent medicines containing Polygonum multiflorum to provide a reference for clinical rational drug use of Polygonum multiflorum and its preparations. One case of long-term taking Jingwu capsule and Huolisu oral liquid, which led to the drug-induced liver injury, was reported. The other case took Runzaozhiyang capsule for a long time, which also led to drug-induced liver injury. Jingwu capsule, Huolisu oral liquid, and Runzaozhiyang capsule all contained Polygonum multiflorum, which could result in liver injury when used long-term. Moreover, we explored the clinical features and toxicity of liver damage induced by Polygonum multiflorum. Liver damage in serum transaminase was significantly increased, and the increasing rate of ALT was more than that of AST. Jaundice appeared obviously. The liver damage mechanisms included drug metabolism, immune response, physical fitness, and many other reasons. Corresponding suggestions on rational use of Polygonum multiflorum and its preparations were presented. The dosage and period should be regulated. The index of liver function should be monitored during the medication periods. Collectively, patients with a history of liver disease or a history of allergies should pay more attention when using the above-mentioned drugs.     

A new dicoumarinoid glycoside from Daphne giraldii

A new dicoumarinoid glycoside, named giraldoid A (1), has been isolated from Daphne giraldii Nitsche. The structure of 1 was determined as 7-O-β-glucosyl-8-(7-hydroxy-2H-1-benzopyran-2-one-8-)yl-2H-1-benzopyran-2-one on the basis of chemical reactions and spectroscopic methods.     

A novel sulphur glycoside from the seeds of Descurainia sophia (L.)

A new sulphur glycoside, named descurainoside (1), and the known compound sinapic acid (2) have been isolated from the seeds of Descurainia sophia (L.) Webb ex Prantl. The structure of 1 has been identified as (1R,6S,8R,9S,10S)-9,10-dihydroxy-4-[(4-hydroxy-3,5-dimethoxyphenyl)methylene]-8-(hydroxymethyl)-2,7-dioxa-5-thiabicyclo[4.4.0]decan-3-one by means of physico-chemical properties and spectroscopic methods (1D and 2D NMR, HRMS, ESI-MS).     

Ether-soluble resin glycosides from the roots of Ipomoea batatas

Two new resin glycosides, batataosides I (1) and II (2), and five known compounds, friedelin (3), scopoletin (4), octadecyl caffeate (5), β-sistosterol (6) and daucosterol (7), were isolated from the roots of Ipomoea batatas. Their structures have been determined based on the chemical and spectral data. Batataosides I and II have novel structures because the core simonic acid B was esterised with cinnamic acid for the first time, and three different substituent esterification groups in one resin glycoside is scarce. The absolute configuration of the aglycone was elucidated to be S by Mosher's method.     

不同炮制辅料对何首乌药效成分含量的影响

目的研究不同炮制辅料对何首乌药效成分含量的影响,为选择何首乌炮制辅料提供依据。方法分别采用5种不同炮制辅料制备制何首乌,高效液相色谱法按照2015年版中国药典中制何首乌成分含量测定方法分别测定制何首乌中二苯乙烯苷、游离蒽醌的含量,比较不同炮制辅料对何首乌中药效成分含量的影响。结果炮制辅料基本都会降低制何首乌中二苯乙烯苷和游离蒽醌的含量。不同炮制辅料制备的制何首乌中二苯乙烯苷含量从高到低依次为空白对照何首乌>米泔水制何首乌>生姜汁制何首乌>甘草汁制何首乌>熟地汁制何首乌>黑豆汁制何首乌,游离蒽醌含量从高到低依次为甘草汁制何首乌>空白对照何首乌>米泔水制何首乌>熟地汁制何首乌>黑豆汁制何首乌>生姜汁制何首乌。不同炮制辅料制备的何首乌中二苯乙烯苷含量均高于2015年版中国药典中的要求,而游离蒽醌含量均未达到2015年版中国药典中的要求。结论不同炮制辅料对制何首乌中药效成分含量的影响不同。     

Effect of ramosetron on short-circuit current response in rat colonic mucosa

We investigated the effects of ramosetron (YM060, (−)-(R)-5-[(1-methyl-1H-indol-3-yl)carbonyl]-4,5,6,7-tetrahydro-1H-benzimidazole monohydrochloride) on the short-circuit current (I_sc) responses to 5-HT receptor agonists in the rat distal colon, and compared its potency to that of other 5-HT₃ receptor antagonists. 5-Hydroxytryptamine (5-HT) concentration-dependently increased I_sc. The I_sc response to 5-HT was partially reduced by tetrodotoxin and ramosetron, and strongly inhibited by GR113808 ([[1-[(2-methylsulphonyl)amino]ethyl]-4-piperidin-yl]methyl 1-methyl-1H-indole-3-carboxylate). 2-Methyl-5-HT and 5-methoxytryptamine also increased I_sc. The former response was inhibited by ramosetron, and the latter was abolished by GR113808. Ramosetron, YM114 (KAE-393, (−)-(R)-5-[(1-indolinyl)carbonyl]-4,5,6,7-tetrahydro-1H-benzimidazole monohydrochloride) and granisetron concentration-dependently antagonized the I_sc responses to 2-methyl-5-HT with reduction in the maximal response at higher concentrations. Apparent pA₂ values for these antagonists were 10.40, 10.37 and 8.99, respectively. Ondansetron produced clear rightward shifts of the concentration-response curves to 2-methyl-5-HT, with a pA₂ value of 8.53. These results suggest that 5-HT increases I_sc through the 5-HT₃ and 5-HT₄ receptors, and that ramosetron is a potent and selective 5-HT₃ receptor antagonist in rat colonic mucosa.     

Studies on the alkaloid constituents of Evodia rutaecarpa (Juss) Benth var. bodinaieri (Dode) Huang and their acute toxicity in mice

Six alkaloids (1-6) have been isolated from the fruits of Evodia rutaecarpa (Juss) Benth var. bodinaieri (Dode) Huang, two of which are new compounds, identified as 2-undecyl-4(1H)-quinolone (4) and 1-methyl-2-undecanone-10'-4(1H)-quinolone (5); the known compounds were identified as rutaecarpine (1), evodiamine (2), 1-methyl-2-undecyl-4(1H)-quinoline (3) and 2-undecanone-10'-4(1H)-quinolone (6). Compounds 1-5 were evaluated for their acute toxicity.     

Studies on chemical constituents of Polygonum perforliatum L

Two new apianen lactones, named as guanyeliaoine I (1) and guanyeliaoine II (2), have been isolated along with seven known compounds from Polygonum perforliatum L. (Chinese name “Guanyeliao”, Berberidaceae). Their structures were deduced on the basis of spectral data and chemical methods.     

Fungal metabolites, PF1092 compounds and their derivatives, are nonsteroidal and selective progesterone receptor modulators

The potential of new nonsteroidal progesterone receptor ligands, the derivatives of PF1092C ((4aR,5R,6R,7S)-6,7-dihydroxy-4a,5,6,7-tetrahydro-3,4a,5-trimethylnaphtho[2,3-b]furan-2(4H)-one) discovered from fungal metabolites, was evaluated. PF1092A ((4aR,5R,6R,7S)-6-acetoxy-7-hydroxy-4a,5,6,7-tetrahydro-3,4a,5-trimethylnaphtho[2,3-b]furan-2(4H)-one) showed good and moderate affinity for porcine and human progesterone receptors in in vitro receptor binding assays, respectively, and partial agonist activity for the progesterone receptor, as determined in assays of two types of progesterone-dependent enzymes in human mammary carcinoma T47D cells. The derivative of PF1092C, CP8481, ((4aR,5R,6R,7S)-6-(2-furancarbonyloxy)-7-hydroxy-4a,5,6,7-tetrahydro-3,4a,5-trimethylnaphtho[2,3-b]furan-2(4H)-one) possessed better affinity for both progesterone receptors and showed less cross-reactivity for other steroid receptors, such as rat androgen receptor, human glucocorticoid receptor, and human estrogen receptor, and was a more potent modulator of the progesterone receptor than PF1092A. CP8400 ((4aR,5R,6R,7S)-6,7-diacetoxy-4a,5,6,7-tetrahydro-3,4a,5-trimethylnaphtho[2,3-b]furan-2(4H)-one) and CP8401 ((4aR,5R,6R,7S)-6,7-dipropionyloxy-4a,5,6,7-tetrahydro-3,4a,5-trimethylnaphtho[2,3-b]furan-2(4H)-one), other derivatives, were indicated to be progesterone receptor antagonists. These results suggest that PF1092 compounds can serve as a new pharmacophore for potent and specific nonsteroidal progesterone receptor modulators.