化妆品中三种紫外吸收剂检测方法的建立

摘 要 目的：建立高效液相色谱法同时分析化妆品中亚苄基樟脑磺酸、樟脑苯扎铵甲基硫酸、4-甲基苄亚基樟脑这3种紫外吸收剂的方法。方法: 化妆品（水基、乳液类）经甲醇-乙腈-醋酸铵水溶液-四氢呋喃（30∶35∶30∶5,v/v）或者（膏霜、粉质类）经乙腈-甲醇-四氢呋喃（30∶20∶50, v/v）涡旋、超声提取后检测;采用Thermo scientific C18（250 mm×4.6 mm,5 μm）色谱柱,以甲醇、乙腈、0.02 mol·K^-1醋酸铵水溶液（冰醋酸调至pH 5.15）为流动相,梯度洗脱,柱温：35℃,流速：1.0 ml·min^-1 ,DAD 检测器,检测波长288 nm、300 nm。结果: 亚苄基樟脑磺酸、樟脑苯扎铵甲基硫酸、4 甲基苄亚基樟脑分别在12.26～98.06 μg·ml^-1（r=0.999 9）、9.31～74.48 μg·ml^-1（r=0.999 9）、6.86～54.88 μg·ml^-1（r=0.999 9）范围内呈良好的线性关系,检出限及定量限范围分别为4.6,6.4,1.6 ng和17.4,15.9,5.5 ng,平均回收率分别为99.2%（RSD=1.58%）、99.8%（RSD=2.38%）、99.2%（RSD=2.03%）（n=36）。结论:本方法简便快捷,重复性良好,结果准确可靠,适用于化妆品中紫外吸收剂的含量测定。     

液相色谱-质谱联用法测定参蛇软膏中雷公藤甲素的含量

摘 要 目的：建立一种液相色谱 质谱联用法测定参蛇软膏中雷公藤甲素的含量。方法: 色谱条件：色谱柱为Agilent TC C18柱（250 mm×4.6 mm,5 μm）,流动相为甲醇-0.1%甲酸水溶液（73∶27,v/v）,流速为0.5 ml·min^-1,柱温为35℃,进样量为2 μl;质谱条件：采用电喷雾离子源(ESI),多反应离子监测（MRM）,正离子检测模式,以甲硝唑为内标,检测雷公藤甲素;监测离子：雷公藤甲素m/z 361.4→43.2,甲硝唑m/z 172.1→128.0。结果: 雷公藤甲素在10～500 ng·mL^-1范围内呈良好的线性关系,r=0.999 9;定量限（LOQ）为9.5 ng·mL^-1;日内和日间精密度（RSD）均小于3%,平均回收率为96.87%（RSD=2.79,n=6）。结论:本方法简单、快速、灵敏、准确,可用于参蛇软膏中雷公藤甲素的含量测定。     

HPLC-FLD法测定聚明胶肽注射液中交联剂残留量

摘 要 目的：建立测定聚明胶肽注射液中残留交联剂1,4 环己烷二异氰酸酯水解产物1,4 环己烷二胺含量的方法。方法: 采用HPLC FLD法,衍生化试剂：丹磺酰氯,色谱柱：YMC C18柱（250 mm×4.6 mm,5 μm）,流动相：甲醇 水（80：〖KG-*2〗20）,检测器：荧光检测器（激发波长：340 nm,发射波长：515 nm）,流速：1.0 ml·min-1,柱温：35℃,进样量：20 μl。 结果:制剂中其他成分无干扰,反式1,4 环己烷二胺在0.282～5.640 μg·ml^-1（r=0.999 9）范围内的质量浓度与其双酰化衍生物峰面积的线性关系良好,顺式1,4 环己烷二胺在0.298～5.960 μg·ml^-1（r=1.000 0）范围内的质量浓度与其双酰化衍生物峰面积的线性关系良好;反式和顺式1,4 环己烷二胺的平均回收率分别为100.32%（RSD=1.52%,n=6）、99.62%（RSD=1.48%,n=6）,测得各批聚明胶肽注射液中的1,4 环己烷二胺总含量均低于5 μg·ml^-1。结论:该分析方法灵敏度高、准确、专属性强,重复性好,可用于测定聚明胶肽注射液中环己烷二胺残留量的测定。     

HPLC法测定姜黄素-槲皮素复方自微乳的载药量和包封率

摘 要 目的：建立HPLC法测定姜黄素 槲皮素复方自微乳（CUR-QUE-SMEDDS）的载药量和包封率。方法: 采用离心法分离游离药物,HPLC法测定药物含量。色谱柱：Purospher STAR LP C18 柱（250 mm×4.6 mm,5 μm）,流动相：乙腈 4%冰醋酸（50∶50）,流速：1.0 ml·min^-1,检测波长：370 nm,柱温：30℃,进样量：10 μl。结果: 姜黄素和槲皮素的线性范围分别为10.728~96.552 μg·mL^-1（r=0.999 8）和1.08~9.72 μg·mL^-1（r=0.999 9）,平均回收率分别为99.98%（RSD=1.46%,n=9）和100.34%（RSD=1.06%,n=9）。CUR QUE SMEDDS中姜黄素和槲皮素的包封率分别为（95.97±0.50）% 和（95.91±2.52）%,载药量分别为（25.82±0.15）mg·g^-1和（1.80±0.05）mg·g^-1。结论:该法准确可靠,快速简便,适用于测定CUR-QUE-SMEDDS的载药量和包封率。     

HPLC波长切换法测定氨咖黄敏胶囊4个成分的含量

摘 要 目的： 建立HPLC波长切换法同时测定氨咖黄敏胶囊中4个成分的含量。方法: 采用Agilent ZORBAX SB C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以乙腈（A）-甲醇（B）-磷酸二氢铵溶液（取0.1 mol·L^-1磷酸二氢铵溶液1 000 ml ,加磷酸1 ml,混匀）（C）为流动相,梯度洗脱,流速1.0 ml·min^-1,柱温 35℃,变换波长时间为（0～9 min ：225 nm;9～38 min ：450 nm）。结果: 采用HPLC波长切换法测定氨咖黄敏胶囊4个成分的含量,线性范围分别为：对乙酰氨基酚24.680～394.900 μg·ml^-1（r=0.999 9）,马来酸氯苯那敏0.201～3.214 μg·ml^-1（r=0.999 9）,咖啡因1.129～18.070 μg·ml^-1（r=0.999 9）,胆红素0.010～0.165 μg·ml^-1（r=0.999 8）;平均回收率分别为：99.25% (RSD=0.46%), 99.29% (RSD=0.32%),99.49% (RSD=0.48%)及99.75% (RSD=0.55%)（n=6）。结论:该法简单,灵敏,准确,重复性好,可用于氨咖黄敏胶囊的含量测定。     

HPLC波长切换法同时测定茵栀祛黄胶囊中7种成分的含量

摘 要 目的：建立HPLC波长切换法同时测定茵栀祛黄胶囊中栀子苷、甘草苷、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量。方法: 采用Waters Sunfire C18（250 mm×4.6 mm,5 μm）色谱柱;流动相：甲醇（A） 0.05%磷酸溶液（B）（梯度洗脱）,流速为1.0 ml·min^-1 ,柱温为25℃,检测波长(0~15 min：在238 nm波长下检测栀子苷和甘草苷;15~50 min：在254 nm波长下检测芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚),进样量为10 μl。结果: 栀子苷、甘草苷、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的线性范围分别为0.13～3.18 μg·ml^-1（r=0.999 8）、0.19～4.84 μg·ml^-1（r=0.999 7）、0.28～7.02 μg·ml^-1（r=0.999 9）、0.13～3.16 μg·ml^-1（r=0.999 9）、0.61～15.27 μg·ml^-1（r=0.999 9）、0.32～8.03 μg·ml^-1（r=0.999 9）、0.39～9.81 μg·ml^-1（r=0.999 9）;平均加样回收率分别为98.84%（RSD=0.74%）、99.34%（RSD=0.86%）、99.54%（RSD=0.30%）、99.56%（RSD=0.80%）、99.85%（RSD=0.41%）、99.57%（RSD=0.70%）、99.64%（RSD=0.30%）（n=9）。结论: 本文建立的HPLC含量测定方法,具有操作简便、专属性高、重复性良好、结果准确可靠的特点,可用于茵栀祛黄胶囊的质量控制。     

离子色谱法测定枸橼酸氢钾钠颗粒中多种成分的含量

摘 要 目的：建立离子色谱法测定枸橼酸氢钾钠颗粒中钠、钾和枸橼酸含量的方法。方法: 钾和钠的色谱条件：采用Dionex IonPac CS12A色谱柱（250 mm×4.6 mm,5 μm）,流动相为0.02 mol·L^-1甲烷磺酸溶液,流速为1.0 ml·min^-1,抑制器为CSRS 300,抑制电流为59 mA,采用抑制型电导检测器,进样量为25 μl。枸橼酸的色谱条件：采用Dionex HPICE AS1离子排斥色谱柱（250 mm×9.0 mm,7.5 μm）,流动相为0.015 mol·L^-1硫酸溶液,流速为0.6 ml·min^-1,检测波长为220 nm,进样量为10 μl。结果: 钠的线性范围为0.82～82.49 μg·ml^-1（r=0.999 9）,平均回收率为98.9%,RSD为0.55% （n=9）;钾的线性范围为1.38～137.89 μg·ml^-1（r=1.000 0）,平均回收率为100.5%,RSD为0.53%（n=9）;枸橼酸的线性范围为0.021～10.600 mg·ml^-1（r=1.000 0）,平均回收率为99.1%,RSD为0.54%（n=9）。结论:本方法简便、快速、准确,可用于枸橼酸氢钾钠颗粒的质量控制。     

HPLC同时测定复方替米沙坦片中主成分含量

摘 要 目的： 建立复方替米沙坦片中两种药物含量测定的HPLC法。方法: 采用菲罗门C₁₈色谱柱(150 mm×4.6 mm, 5 μm),以50 mmol·L^-1磷酸二氢钠溶液(pH 6.0, 0.5%三乙胺) 乙腈(40∶60, v/v)为流动相,流速1.0 ml·min^-1,检测波长254 nm,柱温30℃,进样量20 μl。结果: 替米沙坦与苯磺酸氨氯地平可达到较好分离,替米沙坦的质量浓度在4.0~80.0 μg·mL^-1内（r=0.999 9）,苯磺酸氨氯地平质量浓度在1.0~20.0 μg·mL^-1（r=0.999 9）内与峰面积呈良好的线性关系。替米沙坦和苯磺酸氨氯地平的平均回收率分别为99.90%和100.52% (n=9) ,RSD分别为0.74%和1.48% (n=9)。结论:该方法专属性强、稳定准确,适用于复方替米沙坦片的含量测定。     

HPLC法测定盐酸阿普林定片的含量和有关物质

摘 要 目的： 建立高效液相色谱法同时测定盐酸阿普林定片含量和有关物质的方法。方法: 色谱柱为Waters symmetry C₁₈（150 mm×4.6 mm,5 μm）,流动相为甲醇 0.02 mol·L^-1磷酸二氢钾(用磷酸调节pH至3.0)（50∶50,v/v）,流速为1.0 ml·min^-1,检测波长为254 nm,柱温为35 ℃,进样量为20 μl。结果: 盐酸阿普林定浓度在3.0～22.5μg·mL^-1范围内呈良好的线性关系（r=0.999 8）,平均加样回收率为99.8%(RSD=0.83%, n=9),检测限和定量限分别为60 ng和300 ng。结论:该方法简便、准确,灵敏度高,重复性好,可用于盐酸阿普林定片的质量控制。     

酮康他索乳膏中酮康唑和丙酸氯倍他索含量测定方法的改进

摘 要 目的：建立同时测定酮康他索乳膏中酮康唑和丙酸氯倍他索含量的方法。方法: 采用HPLC法,色谱柱为Kromasil C18（250 mm×4.6 mm,5 μm）柱,流动相为甲醇 0.05 mol·L^-1醋酸钠溶液（用冰醋酸调pH至5.5）,采用梯度洗脱,流速为1.0 ml·min^-1,检测波长为239 nm,柱温为25℃,进样量为10 μl。结果:酮康唑和丙酸氯倍他索分别在160.30 ~1 282.40 μg· mL^-1和4.03~32.24 μg· mL^-1范围内呈良好的线性关系（r均为1.000 0）。平均回收率分别为100.9%（RSD=0.52%,n=9）和100.2%（RSD=0.56%,n=9）。结论:该方法专属性好、灵敏度高、定量准确,可用于酮康他索乳膏中酮康唑和丙酸氯倍他索的含量检测。     

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.