UPLC法快速测定栀子复方制剂中栀子苷和西红花苷-1含量

目的建立快速测定栀子复方制剂复方牛黄消炎胶囊、清胃黄连丸和龙泽熊胆胶囊中栀子苷和西红花苷-1的方法。方法采用UPLC法。色谱柱为BEH C18柱(50mm×2.1mm,1.7μm);流动相:甲醇-水以不同梯度洗脱;流速:0.3mL·min~(-1);检测波长:0~7min为238nm,7~20min为440nm;柱温:30℃;进样量为2μL。结果 3种复方制剂中栀子苷在0.010~1.000mg·mL~(-1)范围内呈良好的线性关系(r=0.999 9),平均回收率分别为98.2%,99.9%和100.3%,RSD分别为1.3%,1.4%和1.0%;西红花苷-1在0.1~10.0μg·mL~(-1)范围内呈良好的线性关系(r=0.999 9)。平均回收率分别为99.6%,97.4%和98.3%,RSD分别为1.3%,1.4%和1.5%。结论栀子苷和西红花苷-1在20min内获得良好分离,该方法简便、准确、快速,可用于栀子复方制剂中栀子苷和西红花苷-1的测定。     

复方芒果苷滴眼液中芒果苷和盐酸小檗碱的鉴别及含量测定

目的 采用TLC定性鉴别复方芒果苷滴眼液中的芒果苷和盐酸小檗碱并用HPLC测定其含量.方法 用C_(18)柱,流动相为乙腈-0.05 mol·L~(-1)磷酸二氢钾缓冲液(28:72),流速1.0 mL·min~(-1),检测波长265 nm,外标法定量.结果 芒果苷和盐酸小檗碱的线性范围均为0.1～1.0 μg,平均回收率分别为101.0%(RSD=2.09%,n=9)、100.6%(RSD=1.87%,n=9).结论 所建方法简便、准确,可用于复方芒果苷滴眼液的质量控制.     

HPLC法测定羚牛角二十五味丸中栀子苷含量

建立高效液相色谱法测定羚牛角二十五味丸中栀子苷含量的方法.采用Hypersol C18色谱柱,流动相为乙腈-水(12:88),检测波长为238nm,流速1.0mL·min-1,柱温为30℃.栀子苷在0.1067～0.6403цg范围内线性关系良好,r=0.9996;平均回收率为99.69%,RSD为0.18%(n=9).本方法简便、准确、重现性好,适用于该药品成分的含量测定.     

HPLC法测定复肾宁片中栀子苷的含量

目的:用高效液相色谱法测定复肾宁片中栀子苷的含量。方法:采用Agilent C_(18)(250 mm×4.6 mm,5μm)色谱柱,以乙腈-水(10:90)为流动相,流速:1.0ml·min~(-1),检测波长为238 nm。结果:栀子苷进样量在0.1446～1.446μg(r= 0.9999)范围内,与峰面积呈良好的线性关系。栀子苷的平均回收率为100.9%,RSD=1.1%(n=6)。结论:本方法简便可靠,专属性强,重现性好,可用于该制剂的质量控制。     

HPLC法测定栀子超微速溶饮片中栀子苷的含量

目的建立高效液相色谱法测定栀子超微速溶饮片中栀子苷含量。方法采用Hypersil ODS2 C18柱(4.6mm×250mm,5μm),流速:1.0mL/min,流动相:乙腈-水(15︰85);检测波长:238nm,柱温30℃。结果栀子苷进样量在0.2026～2.0260μg(r2=0.9999,n=6)范围内与峰面积呈良好线性关系,平均加样回收率为99.94%(RSD=1.28%,n=6)。结论该测定方法简便、准确、灵敏度高,可作为质量控制方法。     

HPLC法测定玛木然止泻胶囊中盐酸小檗碱与没食子酸的含量

目的采用高效液相色谱法测定玛木然止泻胶囊中盐酸小檗碱和没食子酸的含量。方法色谱柱为Ecosil C18色谱柱(250mm×4.6mm,5μm)。盐酸小檗碱流动相为乙腈-0.05mol·L~(-1)磷酸二氢钾溶液(30∶70),检测波长为345nm,流速为1.0mL·min~(-1);没食子酸流动相为甲醇-2mL·L~(-1)磷酸溶液梯度洗脱,检测波长为270nm,流速为1.0mL·min~(-1)。结果盐酸小檗碱和没食子酸分别在0.211~2.109(r=0.999 1)及0.207~2.071μg·mL~(-1)(r=0.999 6)范围内线性关系良好;平均加样回收率分别为98.20%(RSD=2.20%)和102.52%(RSD=1.28%)。结论该方法准确、简便、重复性好,可用于玛木然止泻胶囊的质量控制。     

高效液相色谱法测定江津栀子中栀子苷含量

目的建立测定江津栀子中栀子苷含量的高效液相色谱法。方法色谱柱为UltimateTM C18键合硅胶柱(250 mm×4.6 mm,5μm),流动相为乙腈-水(10∶90),流速1.0 mL/min,温度25℃,检测波长238 nm。结果栀子苷进样量在3.2～11.2μg范围内与峰面积呈良好的线性关系,回归方程为Y=-439 843.76+1 012 294.70 X,r=0.999 2(n=5);平均加样回收率为99.34%,RSD=1.49%(n=6)。结论高效液相色谱法测定江津栀子中栀子苷的含量,操作简便、结果稳定,精密度、重现性、回收率均较好。     

测定栀子金花丸中三种成分的含量及栀子苷的溶出度

目的:建立同时测定栀子金花丸中栀子苷、盐酸小檗碱和黄芩苷含量的方法,并测定丸中栀子苷的溶出度。方法:采用高效液相色谱法,流动相为甲醇-0.1%磷酸溶液,梯度洗脱,流速为0.8 ml/min,检测波长为254 nm;采用《中国药典》中桨法测定栀子金花丸中栀子苷在水中的溶出量,计算累积溶出度。结果:栀子苷在0.007~0.336μg范围内线性关系良好(r=0.999 9),平均回收率为99.7%,RSD为2.5%;盐酸小檗碱在0.013~0.624μg范围内线性关系良好(r=0.999 8),平均回收率为100.2%,RSD为1.7%;黄芩苷在0.010 5~0.630μg范围内线性关系良好(r=0.999 8),平均回收率为99.0%,RSD为2.3%。栀子苷45 min和120 min累积溶出度分别为79.9%和92.7%结论:建立的方法简便、重复性好,可用于栀子金花丸的质量控制。     

HPLC测定小儿退热口服液中栀子苷含量

目的采用HPLC测定小儿退热口服液中栀子苷的含量.方法选用Hypersil C18色谱柱,流动相:乙腈-水(10∶90),检测波长:238 nm,流速:1.0 ml/min,柱温:室温.结果栀子苷线性关系良好(r＝0.9999),平均回收率达96.9%(RSD＝1.33%).     

HPLC法同时测定芩连片中黄芩苷和小檗碱的含量

目的:建立 HPLC 法同时测定芩连片中黄芩苷和小檗碱含量。方法:以芩连片为研究对象,采用 Kromasil ODS(200 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-0.05 mol·L~(-1)磷酸二氢钾溶液-三乙胺(26:74:0.2),流速1.0 mL·min~(-1),检测波长277 nm,柱温为室温。结果:黄芩苷、小檗碱分别在0.0101～0.1217 mg·mL~(-1)(r=0.9997,n=7),0.0114～0.1372 mg·mL~(-1)(r=0.9998,n=7)范围内呈良好线性关系;平均回收率(n=9)分别为98.7%和97.7%。结论:本测定方法简便、快速、准确,为芩连片质量评价提供了依据。     

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.     

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.