高效液相色谱法测定异丙嗪胆汁片中盐酸异丙嗪的含量

目的:建立高效液相色谱法测定异丙嗪胆汁片中盐酸异丙嗪的含量。方法:Diamonsil~(TM)C_(18)色谱柱(250 mm×4.6 mm,5μm,迪马公司);流动相:0.02mol·L~(-1)磷酸二氢钾缓冲溶液(取磷酸二氢钾2.72 g,加水700 mL 溶解,用磷酸调 pH 至3.0,加水至1000 mL)-乙腈-甲醇(55:20:25),流速:1.0 mL·min~(-1),检测波长:249nm,进样量:10μL。结果:盐酸异丙嗪在5.3-84.6μg·mL~(-1)浓度范围内线性关系良好,r=0.9998(n=6),平均回收率为99.90%,RSD=0.62%(n=5)结论:该法简便、灵敏、准确,专属性强,可用于异丙嗪胆汁片的质量控制。     

HPLC法同时测定人体血浆中氟尿嘧啶及其前体药替加氟的浓度

目的:建立同时测定氟尿嘧啶及其前体药替加氟在人体血浆中浓度的 HPLC 方法。方法:以阿昔洛韦为内标,血浆样品用硝酸银(10%)沉淀蛋白质,采用 Zorbax-ODS C_(18)分析柱(4.6 mm×250 mm,5μm),检测波长为265 nm,流动相:0.01 mol·L~(-1)磷酸盐(用2 mol·L~(-1)氢氧化钠溶液调节 pH 为8.0)-甲醇(97:3),流速1.0 mL·min~(-1),柱温为45℃。结果:氟尿嘧啶、替加氟分别在0.1～20μg·mL~(-1)(r=0.9998)和0.2～40μg·mL~(-1)(r=0.9998)浓度范围内线性关系良好,最低检测浓度分别为5和10 ng·mL~(-1),方法回收率分别为97.2%～101.3%和98.3%～102.6%,日内、日间 RSD 小于6%。结论:方法灵敏、快速、准确,并适用于临床上氟尿嘧啶及前体药替加氟浓度监测。     

高效液相色谱法测定烟酸片中烟酸的含量

目的:建立高效液相色谱法测定烟酸片中烟酸的含量.方法:采用高效液相色谱法.色谱柱为Aglient C18(150mm×4.6mm,5μm);流动相为0.02mol · L-1磷酸二氢钾(pH6.8)-乙睛(90∶10);流速为1.0mL· min-1,柱温为28℃,进样量为20μL,检测波长为261 nm.结果:烟酸在5.004～ 100.08μg·mL-范围内呈良好的线性关系,Y=306.9X-0.9327(r =0.9998);平均加样回收率为99.2％,RSD =0.9(n =9).结论:本法简便,准确,重复性好,适用于烟酸片的质量控制.     

HPLC法测定酮洛芬粉针剂中酮洛芬的含量

目的探讨高效液相色谱法(HPLC)测定酮洛芬粉针剂中酮洛芬的含量。方法采用美国Agilent C18色谱柱(200mm×4.6mm,5μm),以0.01mol.L-1磷酸二氢钾溶液(用磷酸调pH至3.5)-甲醇(55∶45)为流动相,流速为1.0mL.min-1,检测波长为256nm。结果酮洛芬在0.005125~0.05125mg.mL-1范围内呈良好的线性关系,r=0.9996(n=6);平均回收率为99.93%,RSD为0.17%(n=5)。结论该方法结果准确,精密度和重现性好,可用于酮洛芬粉针剂的含量测定。     

高效液相色谱法测定酮洛芬凝胶的含量

目的建立HPLC法测定酮洛芬凝胶剂的含量,为质量控制提供有效的分析手段.方法色谱柱为Dikma Technologies DiamonsilTM C18(4.6 mm×250 mm,5 μm);流动相为甲醇-0.05mol·L-1 磷酸二氢钾溶液(73);流速为1.0 mL·min-1;柱温为35℃;检测波长为255 nm.结果制剂中辅料和有关物质对主药无干扰,酮洛芬在1.0～18.0 mg·L-1,r=0.999 7(n=5)范围内呈良好线性关系;平均回收率分别为100.1%(RSD=1.18%),100.68%(RSD=1.24%),99.0%(RSD=0.43%).结论该法操作简便,结果准确、专属性强,可有效控制本品质量.     

HPLC—UV法同时测定复方坎地沙坦酯片中坎地沙坦酯和氢氯噻嗪的含量

目的:建立同时测定复方坎地沙坦酯片中坎地沙坦酯和氢氯噻嗪含量的HPLC-UV法。方法:采用Phenomenex C_(18)(250mm×4.6mm,5μm)色谱柱,流动相为乙腈-0.1mol·L~(-1)磷酸二氢钠溶液(加0.1%三乙胺,磷酸调pH5.0)(65∶35),流速1.0mL·min~(-1),检测波长262nm,柱温35℃。结果:坎地沙坦酯和氢氯噻嗪分别在1.6～32.0μg·mL~(-1)(r=0.9998)和1.2～23.8μg·mL~(-1)(r=0.9999)浓度范围内线性关系良好;平均回收率(n=9)分别为102.1%和100.7%。结论:本文方法准确、快速,适合于复方坎地沙坦酯片的含量测定。     

HPLC法测定三号金龙片中士的宁的含量

目的:采用高效液相色谱法测定三号金龙片中士的宁的含量。方法:采用 Thermo-C_(18)色谱柱(250mm×4.6mm,5μm),以乙腈-0.01mol·L~(-1)庚烷磺酸钠与0.02mol·L~(-1)磷酸二氢钾等量混合溶液(用10%磷酸调节 pH 2.8)(21:79)为流动相,流速为1.0 mL·min~(-1),检测波长为260nm,柱温为室温。结果:士的宁进样浓度在10.5～70μg·mL~(-1)的范围内与峰面积呈良好的线性关系(r=0.9998),回收率(n=5)为98.9%。结论:本方法操作简便,精密度好,结果准确可靠。     

HPLC法测定人血浆中右旋酮洛芬的浓度

目的:建立HPLC法测定人血浆中右旋酮洛芬的浓度。方法:血浆样品以乙醚为萃取剂,萘普生为内标物;采用Shim-pack VP-ODS色谱柱(150 mm×4．6 mm,5μm);流动相为乙腈-5 mmol·L-1磷酸缓冲液(22:78,pH=6．8),流速1．0 ml·min-1;紫外检测波长262 nm。结果:右旋酮洛芬血浆样品的线性范围为0．02-20．00μg·ml-1,r=0．999 9,n=8。萃取回收率和方法回收率分别为72．28％-75．63％和104．0％-107．8％(n=5),日内、日间RSD分别为0．6％-6．2％和2．7％-4．8％(n=5)。结论:本法简便,准确,重现性好。     

高效液相色谱法测定人血清和置换液中美罗培南浓度

目的:建立高效液相色谱法(HPLC)测定人血清和置换液中美罗培南浓度的方法。方法:采用HPLC法,以依利特Hypersil ODS2柱(4.6mm×150mm,5μm)为色谱柱;甲醇-0.01mol·L-1磷酸二氢钾缓冲液(9∶91)为流动相,pH4.91;流速为1.4mL·min-1;检测波长为297nm。结果:血清中美罗培南的标准曲线方程为Y=17.027X-4.7541,r=0.9997,在0.5~80mg·L-1范围内线性关系良好,平均回收率为100.2%,日内,日间RSD均小于7.2%;置换液中美罗培南的标准曲线方程为Y=18.931X 0.8928,r=0.9998,在0.5~80mg·L-1范围内线性关系良好,平均回收率99.2%,日内、日间RSD均小于7.6%。结论:该方法灵敏准确,适用于临床药动学的研究。     

反相高效液相色谱法测定千层纸素的含量和有关物质

目的建立测定千层纸素的含量和有关物质的RP-HPLC方法。方法采用RP-HPLC法,色谱柱为ODS-2(4.6 mm×150 mm,5μm),甲醇-乙腈-10 mmol·L~(-1)磷酸二氢钾(用磷酸调节pH值至2.5)为流动相梯度洗脱,流速1.0 mL·min-1,柱温30℃,检测波长271 nm。结果在含量测定色谱条件下,千层纸素浓度在2.02~20.23μg·m L~(-1)内与峰面积呈良好线性关系(r=1.000,n=6);在有关物质测定色谱条件下,有关物质黄芩素、汉黄芩素、杂质Ⅰ分别在质量浓度0.0197~0.7872μg·m L~(-1)(r=1.000,n=6)、0.0313~0.6250μg·m L~(-1)(r=0.9997,n=6)、0.0818~2.0440μg·m L~(-1)(r=0.9999,n=5)内与峰面积呈良好的线性关系;黄芩素、杂质Ⅰ和各杂质总含量分别为0.11%、0.39%、0.57%。结论本方法灵敏度高、重现性好、准确可靠,可用于千层纸素有关物质的检测分析及质量控制。     

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.