HPLC法同时测定祛瘀止痛合剂中6种成分的含量

目的:建立同时测定祛瘀止痛合剂中芍药苷、柚皮苷、新橙皮苷、三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1含量的方法。方法:采用高效液相色谱法。色谱柱为Waters Xbridge C18,流动相为0.1%磷酸-乙腈(梯度洗脱),流速为1.0 m L/min,检测波长为203 nm,柱温为20℃,进样量为5μL。结果:芍药苷、柚皮苷、新橙皮苷、三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1检测进样量线性范围分别为0.273 4~2.734μg(r=0.999 9)、0.119 1~1.191μg(r=0.999 9)、0.081 5~0.815μg(r=0.999 9)、0.622 8~6.228μg(r=0.999 9)、0.807 2~8.072μg(r=0.999 9)、1.036 4~10.364μg(r=0.999 9);定量限分别为0.082 0、0.029 8、0.028 5、0.436 0、0.403 6、0.310 9μg,检测限分别为0.027 9、0.009 5、0.010 2、0.124 6、0.121 1、0.093 3μg;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为97.85%~100.34%(RSD=0.81%,n=6)、98.14%~101.22%(RSD=1.09%,n=6)、98.42%~102.15%(RSD=1.29%,n=6)、97.77%~100.25%(RSD=0.96%,n=6)、97.32%~99.53%(RSD=0.81%,n=6)、98.28%~101.51%(RSD=1.11%,n=6)。结论:该方法简便快速、稳定可行、重复性好,可用于祛瘀止痛合剂中6种成分含量的同时测定。     

白薇化学成分与药理作用的研究进展

目的:总结白薇化学成分与药理作用的研究进展,为其深入开发与利用提供参考。方法:以"白薇""萝藦科""化学成分""药理作用""生物活性""Cynanchum atratum""Cynanchum versicolor""Asclepiadaceae""Chemical constituents""Pharmacological activity""Biological activities"等为关键词,在中国知网、万方数据、维普网、PubMed、SciFinder、Web of Science等数据库中组合查询2006年7月-2020年8月发表的相关文献,对白薇化学成分及药理作用的研究进行归纳与总结。结果与结论:白薇为萝藦科植物直立白薇C.atratum Bge.或蔓生白薇C.versicolor Bge.的干燥根及根茎,其主要化学成分包括C₂₁甾体皂苷类、挥发油类、生物碱类、芳香类化合物等,如直立白薇苷A、白前苷A、正十六烷酸、9-脱氢安托芬、3,4-二羟基苯乙酮;具有抗炎、抗肿瘤、美白等多种药理作用。然而,现有研究大多集中在直立白薇上,对蔓生白薇的研究较少;对化学成分的研究主要集中在C₂₁甾体皂苷类化合物上,而涉及其他类型化合物的研究不多;有关C₂₁甾体皂苷类的药理活性研究主要集中在单个化合物层面上,而构效关系研究较为少见。因此,为了更好地开发和利用白薇药材资源,有必要进一步对其化学成分、药理作用、作用机制及构效关系等进行深入研究。     

高效液相色谱-蒸发光散射测定血塞通注射液中三七皂苷R1、人参皂苷Rg1、Re及Rb1的含量

目的:用HPLC-ELSD测定血塞通注射液中三七皂苷R1 、人参皂苷Rg1、Re及Rb1的含量.方法:色谱柱填料为氨基键合硅胶,流动相为乙腈-水(80∶20);漂移管温度为90 ℃,载气流速为2.1 L*min-1.结果: 三七皂苷R1 、人参皂苷Rg1、Re及Rb1的线性范围和相关系数分别为:0.30～2.01μg(r=0.999 1)、1.50～9.98 μg(r=0.999 7)、0.45～3.00μg(r=0.999 2) 及1.20～8.03μg(r=0.999 6);回收率(n=6)分别为103.1%(RSD=2.7%)、98.1%(RSD=2.3%)、102.8%(RSD=2.6%)及96.9%(RSD=2.5%).结论:该方法简便、准确、分离效果好,无干扰,可用于血塞通注射液的质量控制.     

HPLC-ELSD同时测定跌打丸中三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1的含量

目的 建立同时测定跌打丸中三七皂苷R₁、人参皂苷Rg₁和人参皂苷Rb1含量的HPLC-ELSD检测方法。方法 采用Phenomenex Kinetex C₁₈色谱柱(100 mm×4.6 mm,2.6 μm),柱温30 ℃,流速0.5 mL·min^-1,流动相为乙腈-水,梯度洗脱,ELSD检测器,漂移管温度110 ℃,载气(空气)体积流量3.0 L·min^-1。结果 三七皂苷R₁、人参皂苷Rg₁、人参皂苷Rb1分别在0.158~3.16 μg(r=0.999 8),0.407~8.14 μg(r=0.999 5),0.446~8.92 μg(r=0.999 9)内呈良好的线性关系,平均加样回收率分别为97.55%(RSD=1.04%),98.09%(RSD=1.03%),97.34%(RSD=0.81%)。结论 该方法简便、快速、准确,可用于跌打丸的质量控制。     

HPLC法测定更年乐片中朝藿定C、淫羊藿苷、川续断皂苷Ⅵ和大花双参苷A

目的建立多波长HPLC梯度洗脱法同时测定更年乐片中朝藿定C、淫羊藿苷、川续断皂苷Ⅵ和大花双参苷A的方法。方法依利特C18柱(250 mm×4.6 mm,5μm);流动相为乙腈–0.1%磷酸溶液,梯度洗脱;检测波长:270 nm(朝藿定C和淫羊藿苷)、210 nm(川续断皂苷Ⅵ)、230 nm(大花双参苷A);体积流量为1.2 m L/min;柱温为室温;进样量20μL。结果朝藿定C、淫羊藿苷、川续断皂苷Ⅵ和大花双参苷A分别在7.14~142.80μg/m L(r=0.999 8)、5.64~112.80μg/m L(r=0.999 6)、6.35~127.00μg/m L(r=0.999 5)、7.90~158.00μg/m L(r=0.999 3)与其峰面积呈良好的线性关系;朝藿定C、淫羊藿苷、川续断皂苷Ⅵ和大花双参苷A的平均回收率分别为99.24%、96.93%、97.81%、98.32%,RSD值分别为1.28%、0.94%、1.24%、1.50%。结论该方法是一种快速、灵敏、准确的分析方法,可作为更年乐片的质量控制方法。     

高效液相色谱梯度洗脱法同时测定保心宁片中3种皂苷含量

目的建立同时测定保心宁片中三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1含量的高效液相色谱梯度洗脱法。方法采用C18柱(250 mm×4.6 mm,5μm),流动相为乙腈(A)-水(B),梯度洗脱(A相0～12 min为19%,12～60 min为19%～36%,60～70 min为36%),检测波长203 nm,流速1.0 mL/min。结果三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1进样量分别在0.764～6.365μg(r=0.999 9),0.633～5.275μg(r=0.999 9)和0.699～5.825μg(r=0.999 9)范围内与峰面积线性关系良好,平均加样回收率分别为101.74%(RSD=2.35%),100.02%(RSD=0.13%)和101.23%(RSD=2.58%)。结论所用方法简单易行、准确可靠,可作为保心宁片的质量控制方法。     

HPLC-ELSD测定复方丹参片中三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1的含量

目的建立复方丹参片中三七皂苷Rl,人参皂苷Rg1及人参皂苷Rb1含量的方法.方法采用HPLC-ELSD方法,Agilent ODS C18柱(250 mm ×4.6 mm,5 μm),流动相为乙腈-水,梯度洗脱,ELSD为栓测器,载气为氮气流速2.0 L·min-1,漂移管温度70℃.结果三七中皂苷R1,人参皂苷Rg1及人参皂苷Rb1的线性范围分别为0.21～2.14μg(r=0.999 8),1.0～10.0μg(r=0.999 3)和0.93～9.28 μg(r=0.999 1),平均回收率(n=5)分别105.7%(RSD 2.O%),100.7%(RSD 1.2%)和101.4%(RSD 1.2%).结论方法简单,快速和准确,用于复方丹参片的质量控制.     

HPLC同时测定左归丸中的5种成分

目的 采用HPLC法同时测定左归丸中尿囊素、薯蓣皂苷元、梓醇、麦角甾苷和吉奥诺苷B1的含量.方法 采用依利特C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.2％磷酸溶液,梯度洗脱,流速1.3 mL· min-1,柱温为30℃,检测波长为224(尿囊素)、210(薯蓣皂苷元和梓醇)和330(麦角甾苷和吉奥诺苷B1)nm.结果 尿囊素、薯蓣皂苷元、梓醇、麦角甾苷和吉奥诺苷B1的线性范围分别为7.270～145.4μg·mL-1(r=0.9999)、5.150～103.0 μg·mL-1(r=0.9992)、5.730～114.6 μg·mL-1(r =0.9998)、6.740 ～134.8 μg·mL-1(r =0.9995)和5.100～102.0 μg·mL-1(r =0.9997);其平均加样回收率分别为98.37％、96.92％、99.11％、96.65％、98.31％,RSD分别为0.89％、1.28％、1.10％、0.57％、1.34％(n=6).结论 所用方法简便快捷、回收率好、重复性好,可用于左归丸中尿囊素、薯蓣皂苷元、梓醇、麦角甾苷和吉奥诺苷B1的含量测定.     

蔓生白薇中白薇新甙的分离和结构鉴定

中药白薇品种比较混乱,据谢宗万等考证,正品白薇应为萝藦科植物直立白薇(Cynanchum atratum Bunge)和蔓生白薇(C.versicolor Bunge)的根。张壮鑫等报道了直立白薇的C_(21)甾体成分,本文报道蔓生白薇的化学成分。     

HPLC法测定复方皂矾丸中西洋参的含量

目的:建立复方皂矾丸中西洋含量测定测方法.方法:采用高效液相色谱法同时测定西洋参中人参皂苷Rg1、人参皂苷Re和人参皂苷Rb1的含量.结果:高效液相色谱人参皂苷Rg1的线性范围是0.63～5.06 μg(r＝0.999 9),平均加样回收率101.12%(RSD＝2.14%),人参皂苷Re的线性范围是1.05～8.4 μg(r＝0.999 8),平均加样回收率100.71%(RSD＝1.57%),人参皂苷Rb1的线性范围是2.468～19.744μg(r＝0.999 7),平均加样回收率97.22%(RSD＝1.92%).结论:该方法操作简便、结果准确、重现性好,可用于复方皂矾丸中西洋参的含量测定.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

Nachweis einiger Heilmittel in der Kniegelenksynovialflüssigkeit

Zusammenfassung Mittels Gaschromatographie und Dünschichtchromatographie wiesen die Autoren 11 Substanzen nach, welche durch Injektion oder nach Verabreichung per os in die Kniegelenksynovialflüssigkeit eindrangen. In ihrer Aufstellung konnten sie eine direkte Beziehung zwischen Struktur sowie chemischphysikalischen Eigenschaften der Substanz und ihrer Fähigkeit, aus dem Blut in die Kniegelenksynovialflüssigkeit einzudringen, nicht nachweisen, außer der Tatsache, daß Substanzen mit starker Affinität zu Eiweißstoffen erst in höheren Dosen nachweisbar waren.     

Lung disease and PKCs

The lung offers a rich opportunity for development of therapeutic strategies focused on isozymes of protein kinase C (PKCs). PKCs are important in many cellular responses in the lung, and existing therapies for pulmonary disorders are inadequate. The lung poses unique challenges as it interfaces with air and blood, contains a pulmonary and systemic circulation, and consists of many cell types. Key structures are bronchial and pulmonary vessels, branching airways, and distal air sacs defined by alveolar walls containing capillaries and interstitial space. The cellular composition of each vessel, airway, and alveolar wall is heterogeneous. Injurious environmental stimuli signal through PKCs and cause a variety of disorders. Edema formation and pulmonary hypertension (PHTN) result from derangements in endothelial, smooth muscle (SM), and/or adventitial fibroblast cell phenotype. Asthma, chronic obstructive pulmonary disease (COPD), and lung cancer are characterized by distinctive pathological changes in airway epithelial, SM, and mucous-generating cells. Acute and chronic pneumonitis and fibrosis occur in the alveolar space and interstitium with type 2 pneumocytes and interstitial fibroblasts/myofibroblasts playing a prominent role. At each site, inflammatory, immune, and vascular progenitor cells contribute to the injury and repair process. Many strategies have been used to investigate PKCs in lung injury. Isolated organ preparations and whole animal studies are powerful approaches especially when genetically engineered mice are used. More analysis of PKC isozymes in normal and diseased human lung tissue and cells is needed to complement this work. Since opposing or counter-regulatory effects of selected PKCs in the same cell or tissue have been found, it may be desirable to target more than one PKC isozyme and potentially in different directions. Because multiple signaling pathways contribute to the key cellular responses important in lung biology, therapeutic strategies targeting PKCs may be more effective if combined with inhibitors of other pathways for additive or synergistic effect. Mechanisms that regulate PKC activity, including phosphorylation and interaction with isozyme-specific binding proteins, are also potential therapeutic targets. Key isotypes of PKC involved in lung pathophysiology are summarized and current and evolving therapeutic approaches to target them are identified.     

Gender-related symptoms and correlates of alcohol dependence among men and women with a lifetime diagnosis of alcohol use disorders

This study explored gender-related symptoms and correlates of alcohol dependence in a crosssectional study of 150 men and 150 women with a lifetime diagnosis of alcohol use disorders (AUD). Participants were recruited in equal numbers from treatment settings, correctional centres and the general community. Standardized measures were used to determine participants' use of substances, history of psychiatric disorders and psychosocial stress, their sensation seeking and family history of substance use and mental health disorders. Multivariate analyses were used to detect patterns of variables associated with gender and the lifetime severity of AUD. Men had a longer history of severe AUD than women. Women had similar levels of alcohol dependence and medical and psychological sequelae as men, despite 6 fewer years of AUD. More women than men had a history of severe psychosocial stress, severe dependence on other substances and antecedent mental health problems, especially mood and anxiety disorders. There were differences in family history of alcohol-related problems approximating same-gender aggregation. The severity of a lifetime AUD was predicted by its earlier age at onset and the occurrence of other disorders, especially anxiety, among both men and women. The limitations in the generalizability of these findings due to sample idiosyncrasies are discussed.     

Biochemical and molecular characterisation of cubozoan protein toxins

Class Cubozoa includes several species of box jellyfish that are harmful to humans. The venoms of box jellyfish are stored and discharged by nematocysts and contain a variety of bioactive proteins that are cytolytic, cytotoxic, inflammatory or lethal. Although cubozoan venoms generally share similar biological activities, the diverse range and severity of effects caused by different species indicate that their venoms vary in protein composition, activity and potency. To date, few individual venom proteins have been thoroughly characterised, however, accumulating evidence suggests that cubozoan jellyfish produce at least one group of homologous bioactive proteins that are labile, basic, haemolytic and similar in molecular mass (42-46 kDa). The novel box jellyfish toxins are also potentially lethal and the cause of cutaneous pain, inflammation and necrosis, similar to that observed in envenomed humans. Secondary structure analysis and remote protein homology predictions suggest that the box jellyfish toxins may act as α-pore-forming toxins. However, more research is required to elucidate their structures and investigate their mechanism(s) of action. The biological, biochemical and molecular characteristics of cubozoan venoms and their bioactive protein components are reviewed, with particular focus on cubozoan cytolysins and the newly emerging family of box jellyfish toxins.     

Dose tolerability of chronically inhaled voriconazole solution in rodents

Invasive pulmonary aspergillosis (IPA) is a fungal disease of the lung associated with high mortality rates in immunosuppressed patients despite treatment. Targeted drug delivery of aqueous voriconazole solutions has been shown in previous studies to produce high tissue and plasma drug concentrations as well as improved survival in a murine model of IPA. In the present study, rats were exposed to 20 min nebulizations of normal saline (control group) or aerosolized aqueous solutions of voriconazole at 15.625 mg (low dose group) or 31.25 mg (high dose group). Peak voriconazole concentrations in rat lung tissue and plasma after 3 days of twice daily dosing in the high dose group were 0.85 ± 0.63 μg/g wet lung weight and 0.58 ± 0.30 μg/mL, with low dose group lung and plasma concentrations of 0.38 ± 0.01 μg/g wet lung weight and 0.09 ± 0.06 μg/mL, respectively. Trough plasma concentrations were low but demonstrated some drug accumulation over 21 days of inhaled voriconazole administered twice daily. Following multiple inhaled doses, statistically significant but clinically irrelevant abnormalities in laboratory values were observed. Histopathology also revealed an increase in the number of alveolar macrophages but without inflammation or ulceration of the airway, interstitial changes, or edema. Inhaled voriconazole was well tolerated in a rat model of drug inhalation.