炮制工艺对何首乌成分的影响

目的 分析不同炮制工艺对何首乌中的二苯乙烯苷、蒽醌、鞣质含量的影响。方法 统计何首乌经不同工艺(黑豆汁蒸片、黑豆汁炖片、黑清蒸片、黑豆汁高压蒸片、黑豆汁屉上蒸片等)炮制12 h、32 h后的二苯乙烯苷含量,不同批次何首乌生片在黑豆汁炖32 h下的二苯乙烯苷与蒽醌含量,不同炮制工艺(生片、豆汁蒸32 h、豆汁炖32 h、清蒸32 h、豆汁高压蒸12 h、豆汁屉上蒸32 h)下炮制的何首乌中蒽醌的含量以及豆汁炖不同炮制时间(0 h、12 h、24 h、36 h、48 h)二苯乙烯苷、蒽醌和鞣质含量。结果 黑豆汁高压蒸片工艺下炮制12 h的二苯乙烯苷含量最高,黑豆汁炖片共一下炮制32 h二苯乙烯苷含量最高;豆汁炖在0 h下二苯乙烯苷含量最高;在生片状态下,来源于广东的三种何首乌中的二苯乙烯苷含量最高,其次为云南,四川和贵州的二苯乙烯苷含量大致相同。在黑豆汁炖32 h下,来自于云南的何首乌片的二苯乙烯苷含量最高,其次为来自于广东的何首生片,然后为来自于贵州的何首乌片,最低的为来自于四川的何首乌片;豆汁高压蒸12 g下游离大黄素含量最高、豆汁蒸32 h下游离大黄素甲醚含量最高、生片状态下,总大黄...     

黑豆汁拌蒸对何首乌中24种成分含量的影响

目的 探究《中华人民共和国药典》（2020年版）收载的黑豆汁拌蒸炮制法,在不同炮制时间（0～48 h）下对何首乌中主要化学成分含量的影响,为何首乌用药安全提供参考。方法 制备药典黑豆汁拌蒸样品;建立超高效液相色谱-三重四极杆质谱分析方法（UPLC-QQQ-MS/MS）,测定何首乌药材中24种成分含量。结果 建立UPLC-QQQ-MS/MS方法,测定何首乌中二苯乙烯苷、蒽醌、黄酮、酚类化合物含量;随着蒸制时间的延长,24种成分的含量发生了明显变化;多数二苯乙烯苷类、蒽醌类、黄酮类经长时间炮制含量降低,酚类成分随炮制时间延长含量增加。结论 本方法操作简单、准确度高、重复性好,可以用于炮制前后何首乌中24种化学成分的定量检测分析。制何首乌中24种成分的含量与蒸制时间密切相关,蒽醌类、二苯乙烯苷类、黄酮类、酚类发生规律性变化,对何首乌毒副作用和补益功效产生重要影响。     

高压蒸制不同时间的何首乌质量标准探讨

目的为制定何首乌合理的炮制工艺提高依据。方法用偏光显微镜观察了淀粉粒在何首乌炮制过程中的变化并比较何首乌各炮制品的蒽醌类成分、总糖、卵磷脂、二本乙烯苷、水溶性浸出物的含量。结果采用同一种炮制方法炮制,随着蒸制时间增加,水溶性浸出物的含量不断增加,何首乌中结合蒽醌含量越来越低,游离蒽醌、总糖、卵磷脂等成分的含量在一定蒸晒时间范围内随着蒸晒时间的增多而增加,二苯乙烯苷的含量随着蒸晒时间的增加而逐渐降低,以高压锅蒸7h含量最高,随后各成分的含量有所下降。结论何首乌作为补益药应用时采用高压蒸7h炮制品较好。用偏光显微镜观察了淀粉粒在何首乌炮制过程中的变化,能有效控制何首乌炮制品的质量。     

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。     

炮制对何首乌中有效成分含量的影响

目的 :测定何首乌炮制前后蒽醌类和二苯乙烯苷的含量变化。方法 :大黄素对照品溶液与 0 .5 %Mg(AC) 2 显色 ,在5 10nm处以 0 .5 %Mg(AC) 2 为空白 ,测其吸收度 ;二苯乙烯苷对照溶液以 95 %乙醇稀释定容 ,在 310nm处测其吸收度。结果 :大黄素和二苯乙烯苷测定回归方程分别为Y =2 9.70X +7.95× 10 -3 ,r =0 .9993和Y =73.0 0X +0 .0 4 2 0 ,r =0 .99992。结论 :制何首乌中游离蒽醌的含量略高于生何首乌 ,而结合蒽醌的含量生何首乌则明显高于制何首乌 ;二苯乙烯苷的含量生何首乌要高于制何首乌     

不同炮制工艺对何首乌中二苯乙烯苷含量的影响

目的 考察炮制工艺和炮制时间对何首乌中2,3,5,4-四羟基二苯乙烯-2-O-β-D-葡萄糖苷(二苯乙烯苷)含量的影响.方法 将何首乌分别采用黑豆汁拌蒸0、2、4、6、8、10 h和传统工艺(九蒸九晒)炮制后,用HPLC测定炮制饮片中二苯乙烯苷的含量.结果 不同炮制工艺的饮片中二苯乙烯苷含量顺序为传统工艺炮制品＞生品＞黑豆汁拌蒸品.用黑豆汁拌蒸,二苯乙烯苷的含量先逐渐上升而后下降,以6 h为峰.结论 应规范何首乌饮片的炮制时间.     

Box-Behnken响应面法优化高压蒸法炮制何首乌工艺

摘 要 目的：通过Box-Behnken响应面法优化高压蒸法炮制何首乌工艺,并与传统炮制工艺进行比较。方法: 以蒸制温度、蒸制时间和干燥温度作为考察因素,以多糖含量、二苯乙烯苷含量和两指标归一化值作为评价指标,采用Box-Behnken响应面法考察了各个因素对高压法炮制工艺何首乌中多糖和二苯乙烯苷含量的影响,并比较高压蒸法炮制品与传统炮制品中多糖和二苯乙烯苷含量的差异。结果:高压蒸法炮制何首乌的最佳工艺为：蒸制温度为125.4 ℃、蒸制时间为3.1 h、干燥温度为52 ℃。优化的高压蒸法炮制的何首乌中多糖和二苯乙烯苷含量分别为传统炮制法的1.24和5.26倍。结论:利用Box-Behnken响应面法优化高压法炮制何首乌,方法简便,预测性良好。     

炮制时间对何首乌中蒽醌含量的影响

目的考察炮制时间对何首乌中蒽醌含量的影响。方法何首乌分别用黑豆汁拌蒸2、4、6、8、10h,采用直接醋酸镁比色法和酸水解后醋酸镁比色法,分别测定炮制饮片中游离蒽醌和总蒽醌的含量。结果黑豆汁拌蒸品随炮制时间的变化游离蒽醌含量逐渐升高,但总蒽醌没有显著性变化。结论应规范何首乌饮片的炮制时间,使何首乌有效成分可控。     

清炒法炮制粉葛过程中主要化学成分与工艺、物性及颜色变化的相关性分析

目的：研究清炒法炮制过程中粉葛主要化学成分与工艺、物性及颜色的动态变化,以及其相关性。方法：测定不同炮制阶段粉葛样品的物性参数（氧化值、膨胀度、堆密度、pH值）,利用影像设备、Photoshop软件等获取炮制品图片的颜色变化值,采用紫外分光光度苯酚-硫酸显色法测定粉葛中可溶性多糖的含量,运用双波长法测定粉葛中总淀粉含量,最后对参数进行配对样本t检查、方差分析及线性回归分析。结果：随着炮制程度的加强,粉葛中总淀粉含量降低,水溶性多糖的含量先增高再降低,两者呈负相关。粉葛中可溶性多糖的含量与氧化性、红-绿色轴值呈明显正相关性,与膨胀度成明显负相关,淀粉含量与堆密度呈明显负相关。主要化学成分与部分物性参数及色度值线性回归显著。结论：粉葛在清炒法炮制过程中,参数间可能存在转化。部分颜色变化和物性参数数据可以作为评价炮制程度及合格与否的标准,弥补传统人为判断造成炮制品质量无法统一的不足,从而规范生产工艺。     

HPLC法测定不同产地生何首乌和不同炮制工艺制首乌中顺（反）式二苯乙烯苷含量

目的 比较不同产地何首乌及不同炮制工艺制何首乌中顺(反)二苯乙烯苷含量的变化,探究其炮制减毒增效的作用机制,为何首乌质量控制及饮片炮制标准研究提供数据参考,以期降低临床用药风险。方法 采用高效液相色谱法,测定何首乌和制何首乌中顺(反)式二苯乙烯苷(2,3,5,4′-四羟基二苯乙烯-2-O-β-D-葡萄糖苷)的含量。结果 不同批次何首乌和制何首乌中顺(反)式二苯乙烯苷含量范围分别为27.23～358.19μg·g^-1和10.30～52.00 mg·g^-1。结论本方法操作简单,准确度高,重复性好,可以用于何首乌和制何首乌中顺(反)式二苯乙烯苷含量测定。     

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.     

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.