HPLC测定兔血浆中的藁本内酯

目的 采用HPLC测定兔血浆中藁本内酯的浓度.方法 样品经正己烷萃取后进样分析.色谱柱为Kromasil C18(150mm×4.6 mm,5 μm),流动相为甲醇-水(75:25),流速1.0 ml·min-1,检测波长328 nm,测定兔灌胃100 mg·kg-1当归挥发油有效部位后的血药浓度变化.结果 藁本内酯在血浆中的线性范围为0.2～6.4 μg·ml-1,最低检测浓度为0.1 μg·ml-1,日内和日间RSD均小于8%,平均回收率分别为97.18%、93.91%.兔灌胃后,Tpeak=1.28±0.12 h,Cmax=3.86±0.24 μg·ml-1,t1/2α=2.04±0.20 h.结论 所建方法符合生物样品的测定要求,可用于兔血浆中藁本内酯的测定和药物动力学研究.     

复方当归微乳中桂皮醛和藁苯内酯的含量测定

目的 建立高效液相色谱(HPLC)法测定复方当归微乳中主成分藁苯内酯和桂皮醛的含量,为其质量标准的建立提供依据. 方法 色谱柱为Inertsil ODS 3柱(4.6 mm×150 mm,5 μm),流动相为乙腈-水(55：45),流速1.0 mL.min^-1,检测波长：285 nm,柱温30 ℃. 结果桂皮醛在0.484 5～38.750 0 μg.mL^-1浓度范围内呈良好的线性关系,回归方程为Y＝27.060X-1.586 (r＝0.999 8),加样回收率为99.60%,日内和日间精密度RSD低于1.25%;藁本内酯在0.531 0～106.100 0 μg.mL^-1范围内线性关系良好,回归方程为Y＝13.930X＋1.344(r＝0.999 8),加样回收率为98.92%,日内和日间精密度RSD低于1.25%. 结论 建立的HPLC法专属性强、灵敏度高,可用于复方当归微乳的质量控制.     

祛腐再生膏的质量标准研究

目的:提高祛腐再生膏的质量标准,更好地控制产品质量。方法 :采用薄层色谱法(TLC)对该制剂中当归和白芷药材进行定性鉴别;采用高效液相色谱法(HPLC)测定制剂中藁本内酯的含量,色谱条件:色谱柱为Diamonsil C18柱(200 mm×4.6 mm,5μm);流动相为甲醇-0.05%三氟乙酸水(58∶42);流速为1.0 mL.min-1;检测波长为328 nm;柱温为30℃。结果:薄层色谱法可检出当归和白芷,斑点清晰,分离度好,阴性无干扰;藁本内酯在0.040 6~2.03μg范围内与峰面积呈良好的线性关系(r=0.999 8),藁本内酯的平均回收率为98.26%,RSD=2.48%(n=9)。结论:本文方法简便、专属性好、准确,可作为祛腐再生膏的质量控制标准。     

RP-HPLC法测定自微乳中雷公藤红素的含量

目的:建立测定自微乳制剂中雷公藤红素含量的HPLC方法.方法:采用RP-HPLC法,色谱柱为Inertsil ODS-3C18,流动相为甲醇-乙腈-1％甲酸溶液(85∶10∶5),流速为1.0 ml·min-1,紫外检测波长为425 nm,柱温为35℃,进样量为20 μl.结果:雷公藤红素与辅料及溶剂峰分离良好,雷公藤红素在1.0～100 μg·ml-1范围内线性关系良好,回归方程为:Y=5141.09X-7 116.88(r=0.999 9);加样回收率分别为102.06％、102.03％和97.90％,日内、日间RSD均＜1.0％.结论:该方法简便快速、准确、重现性好,能有效测定自微乳制剂中雷公藤红素的含量.     

紫外分光光度法测定川芎油中的总内酯

目的 采用紫外分光光度测定川芎油中的总内酯.方法 以藁本内酯作对照品,样品和对照品中加入4 ml 30 mg·ml-1的NaOH溶液,30℃保温反应30 min后,于305 nm测定吸光度.结果 藁本内酯2.95～23.6 μg·ml-1与吸光度呈良好的线性关系,其同归方程为:Y=36.8X+0.009(r=0.9998),总内酯的平均回收率为98.1%,RSD=1.1%.3批川芎油含量测定的结果分别为51.3%、53.0%、57.5%.结论 所建方法可以作为川芎油中总内酯的含量测定方法.     

HPLC测定复方穿心莲片中穿心莲内酯和脱水穿心莲内酯的含量

目的 建立测定复方穿心莲片中穿心莲内酯和脱水穿心莲内酯含量的方法。方法 采用HPLC法,色谱柱为Diamonsil-C18柱,甲醇-水(70∶30)为流动相,流速1.0 ml·min-1,检测波长225 nm,柱温为室温。结果 穿心莲内酯、脱水穿心莲内酯的平均回收率分别为96.6％、96.8％,分析方法精密度(RSD)分别为1.83％和1.50％(n=6)。结论 所用方法简便、准确,能有效地控制该制剂的质量。     

HPLC测定复方木香小檗碱片中的木香烃内酯

目的 测定不同批次复方木香小檗碱片中木香烃内酯的含量.方法 采用HPLC法,色谱柱为Kromasil C18 (250 mm×4.6 mm,5μm),流动相为甲醇-水(70∶30),检测波长225 nm,流速1.0 mL· min-1,柱温25℃,进样体积10 μL.结果 木香烃内酯10.78～107.8 μg· mL-1与峰面积呈良好的线性关系(r=0.9999,n=9),平均加样回收率为99.86％,RSD=1.4％(n=9);5批次复方木香小檗碱片中的木香烃内酯的含量为0.08％.结论 所用方法简单、稳定,木香烃内酯的含量可作为复方木香小檗碱片的品质评价依据之一.     

高效液相色谱法测定川芎内酯软胶囊中4种苯酞成分

目的建立高效液相色谱法同时测定川芎内酯软胶囊中苯酞类化学成分洋川芎内酯-Ⅰ、洋川芎内酯-H、瑟丹酸内酯、藁本内酯的含量。方法 Shiseido Capcell Pak C18 MGⅡ色谱柱(4.6 mm×150 mm,5μm),流动相:甲醇-0.5%冰醋酸溶液,梯度洗脱,流速:0.7 m L·min-1,柱温:30℃,检测波长为280 nm,进样量:10μL。结果 4个化合物与周围干扰峰达到基线分离,线性范围分别为洋川芎内酯-Ⅰ0.193 3⁴.832μg·m L-1(r=0.993 8);洋川芎内酯-H 0.080 644.832μg·m L-1(r=0.993 8);洋川芎内酯-H 0.080 64².016μg·m L-1(r=0.999 8);瑟丹酸内酯3.4152.016μg·m L-1(r=0.999 8);瑟丹酸内酯3.415⁸5.38μg·m L-1(r=0.999 8);藁本内酯11.7985.38μg·m L-1(r=0.999 8);藁本内酯11.79²94.7μg·m L-1(r=0.999 2)。RSD均<2%(n=6),平均加样回收率在95%294.7μg·m L-1(r=0.999 2)。RSD均<2%(n=6),平均加样回收率在95%¹02%(n=6)。川芎内酯软胶囊中洋川芎内酯-Ⅰ、洋川芎内酯-H、瑟丹酸内酯、藁本内酯的含量分别为0.335 0、0.112 0、6.208、16.84 mg·g-1(n=3)。结论该法简便、快捷、结果准确、重复性好、实用性强,可用于川芎内酯软胶囊的质量控制。     

双波长HPLC法同时测定止痢宁片中穿心莲内酯和脱水穿心莲内酯的含量

目的:建立高效液相色谱法同时测定止痢宁片中穿心莲内酯和脱水穿心莲内酯含量的方法.方法:色谱柱:CAPCELL PAK-C18柱(150 mm×4.6 mm,5 μm);流动相:甲醇-水(48:52);流速为1.0 ml·min-1;柱温:30℃;检测波长:225 nm(穿心莲内酯)、250 nm(脱水穿心莲内酯);进样量:5 μl.结果:穿心莲内酯在4.17～41.68 μg·ml-1 (r=0.999 9)、脱水穿心莲内酯在4.04～40.40 μg·ml-1(r=0.999 9)浓度范围内线性关系良好;穿心莲内酯回收率为99.21%(RSD=1.3%,n=6),脱水穿心莲内酯回收率98.73%(RSD=1.1%,n=6).结论:该方法简单、准确,可作为止痢宁片的质量控制.     

HPLC法测定圣愈汤冻干粉中4个指标成分的含量

目的:建立测定圣愈汤冻干粉中阿魏酸、毛蕊花糖苷、藁本内酯、黄芪甲苷含量的方法。方法:采用高效液相色谱法测定3批冻干粉样品4种成分含量。测定阿魏酸、毛蕊花糖苷、藁本内酯的色谱柱为Inertsil ODS-SP C_(18),流动相为甲醇-0.1%磷酸水溶液,梯度洗脱,流速为1.0 mL/min,检测波长为330 nm,检测器为二极管阵列检测器,柱温为30℃,进样量为10μL;测定黄芪甲苷的色谱柱为Kromasil C_(18),流动相为乙腈-水(32∶68,V/V),检测器为蒸发光散射检测器,漂移管温度为100℃,载气(空气)流量为2.5 L/min,流速为1.0 mL/min,柱温为30℃,进样量为10μL。结果:阿魏酸、毛蕊花糖苷、藁本内酯和黄芪甲苷进样量线性范围分别为0.050 15～10.03μg(r=0.999 8)、0.067 80～13.56μg(r=0.999 9)、0.057 30～11.46μg(r=0.999 5)、1.128～11.28μg(r=0.999 3);检测限分别为2.12×10~(-4)、1.30×10~(-3)、8.02×10~(-4)、1.09×10~(-3)μg,定量限分别为7.43×10~(-4)、3.87×10~(-3)、2.34×10~(-3)、3.36×10~(-3)μg;精密度、稳定性(12 h)、重复性试验的RSD均小于2%(n=6);平均加样回收率分别为99.6%(RSD=0.83%,n=6)、100.9%(RSD=1.07%,n=6)、98.8%(RSD=0.84%,n=6)和101.3%(RSD=0.99%,n=6)。3批样品中阿魏酸、毛蕊花糖苷、藁本内酯和黄芪甲苷的含量分别为1.225～1.248、0.413～0.424、0.325～0.332、0.394～0.404 mg/g(批间RSD<1.5%)。结论:建立的含量测定方法稳定性、重复性好,能够快速、准确地测定圣愈汤冻干粉中阿魏酸、毛蕊花糖苷、藁本内酯和黄芪甲苷的含量。     

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.