ICP-MS法同时测定半夏糖浆中6种重金属元素的含量

摘 要 目的：建立电感耦合等离子体质谱法（ICP MS）同时测定半夏糖浆中铅、镉、砷、汞、铜、铬6种重金属元素含量的分析方法。方法: 微波消解法处理样品,用ICP MS法（射频功率1.5kW,采样深度10 mm,等离子气、辅助气和载气流量分别为15.0,0.8,0.7 L·min-1,积分时间为0.3~2 s）检测不同厂家不同批次半夏糖浆中6种重金属元素的含量。结果: 各待测元素线性关系良好,r均≥0.997 0,检出限范围为0.3～15.2 ng·g-1,加样回收率为90.4%～98.7%,RSD≤5.8%。结论: 本方法准确、灵敏、简便,可用于半夏糖浆中6种重金属元素的含量测定。     

ICP-MS测定一次性使用重力输液式输液器及静脉输液针中5种重金属元素的残留量

摘 要 目的： 建立一次性使用重力输液式输液器及静脉输液针中镉、铬、铜、锡、铅5种重金属元素的含量测定方法。方法: 样品经过预处理,用1%硝酸浸泡,得到样品溶液后用电感耦合等离子体质谱（ICP MS）测定镉、铬、铜、锡、铅5种重金属元素的含量。结果: 在设定的ICP MS测定条件下,5种元素的线性范围均为0～50 ng·mL^-1 (r＞0.999 0)。一次性使用重力输液式输液器和一次性使用静脉输液针,加标回收率分别在92%～116%和1.6%～2.9%范围内(RSD<3,n=9)。结论:该方法操作简便,能够满足一次性使用重力输液式输液器及静脉输液针中重金属元素测定的要求。     

菊花及水煎液中21种金属元素的分析与评价

摘 要 目的：比较6个不同产区菊花中21种重金属元素含量的差异,建立菊花重金属元素的基础数据库,评价菊花服用的安全性。方法: 采用微波消解电感耦合等离子体质谱法（ICP MS）,对33批菊花药材及水煎液样品中铅、镉、砷、汞、铜等21种金属元素的含量进行测定。结果:各元素呈现良好的线性关系（r＞0.997）,回收率在70.0%～118.9%,RSD在0.97%～20.82%,表明该方法准确可靠。33批菊花中有7批镉超过0.3 mg·kg^-1,但水煎液重金属残留均在安全范围。结论:在重金属残留方面菊花汤剂或茶饮方式服用较安全。     

ICP-OES法同时测定右旋糖酐铁中铅、镉、砷、汞等8种重金属元素的含量

摘 要 目的：建立用电感耦合等离子体发射光谱法（ICP OES）同时测定右旋糖酐铁中铅、镉、砷、汞、钴、钒、硒、钼8种重金属元素含量的分析方法。方法: 通过检测波长考察,确定检测波长为：铅220.353 nm、镉228.802 nm、砷188.980 nm、汞194.164 nm、钴228.615 nm、钒311.070 nm、硒196.026 nm、钼204.598 nm。通过仪器参数优化,确定最优高频入射功率为1.3 kW,雾化气流速为0.7 L·min^-1,泵速为10 r·min^-1。应用上述检测参数,采用ICP OES法测定8种重金属元素的含量。结果: 各待测元素线性关系良好,r均大于0.999 0,检出限为0.12~7.26  ng·ml^-1,定量限为0.40~23.96 ng·ml^-1,加样回收率在94.1%~103.4%,RSD均小于3%（n=9）。结论:该方法专属性好,灵敏度高,迅速准确,可用于右旋糖酐铁中8种重金属元素含量的同时测定。     

微波消解-电感耦合等离子体质谱法测定动物类中药中的5种有害元素

摘 要 目的：建立微波消解 电感耦合等离子体质谱法（ICP MS）测定动物类中药中的Pb、Cd、As、Hg、Cu等5种有害元素的方法。方法: 样品经HNO3 H2O2微波消解后,优化了电感耦合等离子体质谱仪工作参数,基体干扰和质谱干扰分别通过使用Ge、In、Bi内标溶液和碰撞反应池技术（KED模式）消除。结果: 5种有害元素的检出限在0.04～0.52 μg·L-1,方法精密度（RSD）为1.1%～4.8%,回收率为92.4%～110.0%。利用本方法对40批次的动物类中药中的5种有害元素进行了测定,结果表明某些动物类中药的有害元素含量较高。结论: 本方法快速灵敏准确,适用于动物类中药中的有害元素的分析。     

消白胶囊质量标准研究

摘 要 目的： 建立消白胶囊的质量标准。方法: 采用薄层色谱法对菟丝子、当归、白芍进行定性鉴别;建立补骨脂素、异补骨脂素的高效液相色谱含量测定方法。结果: 定性鉴别阴性无干扰,分离度高;补骨脂素线性范围为1.082～108.200 μg·mL^-1(r=0.999 8),平均回收率为99.82%,RSD=1.16%。异补骨脂素线性范围为0.818～81.800 μg·mL^-1(r=0.999 7),平均回收率为99.85%,RSD=1.81%。结论: 所建立的质量标准方法可行,可用于消白胶囊的质量控制。     

HPLC法同时测定蛇胆追风丸中阿魏酸、蛇床子素的含量

摘 要 目的： 采用HPLC法同时测定蛇胆追风丸中阿魏酸、蛇床子素的含量。方法: 采用Phenomenex Synergi C₁₈(250 mm×4.6 mm,4 μm)色谱柱,流动相为甲醇 0.1%磷酸,梯度洗脱,检测波长为322 nm,流速为1.0 ml·min^-1。结果: 阿魏酸、蛇床子素线性范围分别为1.244～14.928 μg·ml^-1(r＝0.999 9)、5.004～25.020 μg·ml^-1(r＝0.999 8),平均加样回收率分别为98.3%(RSD=1.4%,n=6)、98.2%(RSD=1.6%,n=6)。结论: 该方法操作简便,结果准确可靠,可作为蛇胆追风丸中阿魏酸、蛇床子素的含量测定方法。     

福林酚法与考马斯亮蓝法测定甘露聚糖肽口服溶液中蛋白质含量的比较

摘 要 目的：分别建立福林酚法与考马斯亮蓝法测定甘露聚糖肽口服溶液中蛋白质含量并做比较。方法: 分别对两种方法的检出限、线性范围进行考察,并进行精密度、重复性、回收率和样品含量的测定。结果: 福林酚法检出限为0.2 μg,蛋白质浓度线性范围为0~112.0 μg(r=0.999 0),平均回收率为105.2%（RSD=1.9%）,精密度RSD均<1% ,样品测定结果分别为47.45,58.34,40.99 μg·ml^-1。考马斯亮蓝法检出限为0.8 μg,蛋白质浓度线性范围0~99.6 μg(r=0.998 0),平均回收率为102.0%（RSD=2.7%）,精密度RSD均<1%,样品测定结果均为未检出。结论: 福林酚法测定甘露聚糖肽口服溶液中蛋白质含量可靠而有效。     

氨咖麻敏胶囊中对乙酰氨基酚、咖啡因、盐酸伪麻黄碱和马来酸氯苯那敏的含量测定

摘 要 目的： 优化测定氨咖麻敏胶囊中各组分含量的方法。方法: 色谱柱为CNW C₁₈（150 mm×4.6 mm,5 μm）,以磷酸二氢铵溶液 乙腈-甲醇（85∶5∶10）为流动相,检测波长为210 nm,同时测定对乙酰氨基酚、盐酸伪麻黄碱、咖啡因含量;色谱柱为CNW C₁₈（250 mm×4.6 mm,5 μm）,以磷酸二氢铵溶液 乙腈（73∶27）为流动相,检测波长为261 nm,测定马来酸氯苯那敏含量。结果: 氨咖麻敏胶囊中对乙酰氨基酚、咖啡因、盐酸伪麻黄碱、马来酸氯苯那敏的线性范围分别为0.100 0～1.000 0 mg·mL^-1（r=0.999 5）、0.012 0～0.120 0 mg·mL^-1r=0.999 9、0.012 0～0.120 0 mg·mL^-1（r=1.000 0）、0.015 0～0.180 0 mg·mL^-1（r=1.000 0）,平均回收率分别为99.9%、101.0%、99.4%、100.0%,RSD分别为1.6%、1.2%、1.7%、1.4%（n=9）。结论: 本方法灵敏度高、专属性强,可用于测定氨咖麻敏胶囊中各组分的含量。     

微波消解-电感耦合等离子体质谱(ICP-MS)法测定棓丙酯原料药中的金属元素

摘 要 目的：建立测定棓丙酯原料药中镁（Mg）、铝（Al）、铬（Cr）、锰（Mn）、镍（Ni）、铁（Fe）、铜（Cu）、锌（Zn）、镉（Cd）等常见金属元素含量的方法。方法: 样品加入硝酸经微波消解处理,采用电感耦合等离子体质谱法以7锂（Li）、45钪（Sc）、72锗（Ge）、115铟（In）为内标元素测定金属元素。测定条件：射频功率为1 530 W,碰撞气为氦气,载气为氩气,载气流量为1.08 L·min-1,积分时间为0.1 s,数据采集重复次数为3次。结果: 各元素在1～200 ng·ml-1范围内线性良好（r＞0.999 0）;检测限为0.003 8～0.785 1 ng·ml-1;精密度、稳定性、重复性的RSD＜5%;各元素平均加样回收率为97.45%～105.24%,RSD为1.1%~3.3%（n=9）。结论: 该方法线性回归良好、灵敏度高、准确性好,适用于棓丙酯原料药中痕量金属元素的检测分析。     

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.     

Efficacy of gut lavage,hemodialysis, and hemoperfusion in the therapy of paraquat or diquat intoxication

Clinical and in vitro investigations were carried out to test the efficacy of gut lavage, hemodialysis, and hemoperfusion in the treatment of poisoning with paraquat or diquat. In a patient suffering from diquat intoxication 130 times more diquat was removed by gut lavage 30 h after ingestion than was removed by complete aspiration of the gastric contents.Determination of in vitro clearances for paraquat and diquat by hemodialysis showed that, at serum concentrations of 1–2 ppm, such as are frequently encountered in poisoning in man, toxicologically relevant quantities of herbicide cannot be removed from the body. At a concentration of 20 ppm, on the other hand, hemodialysis proved to be effective, the clearance being 70 ml/min at a blood flow rate of 100 ml/min. The efficacy of hemoperfusion with coated activated charcoal was on the whole better. Especially at concentrations around 1–2 ppm, the clearance values for hemoperfusion were some 5–7 times higher than those for hemodialysis.In a patient suffering from paraquat poisoning, both hemodialysis as well as hemoperfusion were carried out. The in vitro results could be confirmed: At serum concentrations of paraquat less than 1 ppm no clearance could be obtained by hemodialysis while by hemoperfusion with activated charcoal quite high clearance values were measured and the serum level dropped down to zero.

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Zusammenfassung Klinische Untersuchungen und Laboratoriumsversuche wurden durchgeführt, um die Wirksamkeit von Darmspülung, Hämodialyse und Hämoperfusion bei Paraquat- und Deiquat-Vergiftungen zu prüfen.Bei einem Patienten wurde 30 Std nach Deiquat-Aufnahme durch Darmspülung 130mal mehr Deiquat entfernt als durch vollständige Aspiration des Mageninhaltes. In vitro-Versuche ergaben, daß bei Blutserumkonzentrationen von 1–2 ppm, die bei Vergiftungen oft gemessen werden, durch Hämodialyse keine toxikologisch relevanten Paraquat- oder Deiquat-Mengen entfernt werden können. Dagegen erwies sich die Hämodialyse bei 20 ppm und einer Blutumlaufgeschwindigkeit von 100 ml/min mit einer Clearance von 70 ml/min als wirksam. Die Hämoperfusion mit beschicheter Aktivkohle war in diesen Versuchen aber eindeutig überlegen, denn insbesondere bei Konzentrationen um 1–2 ppm waren die Clearance-Werte 5–7mal höher als bei der Hämodialyse.Die in vitro-Ergebnisse wurden bei einem Patienten mit einer Paraquat-Vergiftung bestätigt: Bei Konzentrationen unter 1 ppm war die Hämodialyse wirkungslos, während durch Hämoperfusion relativ hohe Clearance-Werte erreicht wurden, so daß der Serumspiegel rasch unter die Nachweisgrenze abfiel.

     

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.     

Aquatic Insects and Trace Metals: Bioavailability,Bioaccumulation, and Toxicity

Abstract

The uptake of metals from food and water sources by insects is thought to be additive. For a given metal, the proportions taken up from water and food will depend both on the bioavailable concentration of the metal associated with each source and the mechanism and rate by which the metal enters the insect. Attempts to correlate insect trace metal concentrations with the trophic level of insects should be made with a knowledge of the feeding relationships of the individual taxa concerned. Pathways for the uptake of essential metals, such as copper and zinc, exist at the cellular level, and other nonessential metals, such as cadmium, also appear to enter via these routes. Within cells, trace metals can be bound to proteins or stored in granules. The internal distribution of metals among body tissues is very heterogeneous, and distribution patterns tend to be both metal and taxon specific. Trace metals associated with insects can be both bound on the surface of their chitinous exoskeleton and incorporated into body tissues. The quantities of trace meals accumulated by an individual reflect the net balance between the rate of metal influx from both dissolved and particulate sources and the rate of metal efflux from the organism. The toxicity of metals has been demonstrated at all levels of biological organization: cell, tissue, individual, population, and community. Much of the literature pertaining to the toxic effects of metals on aquatic insects is based on laboratory observations and, as such, it is difficult to extrapolate the data to insects in nature. The few experimental studies in nature suggest that trace metal contaminants can affect both the distribution and the abundance of aquatic insects. Insects have a largely unexploited potential as biomonitors of metal contamination in nature. A better understanding of the physico-chemical and biological mechanisms mediating trace metal bioavailability and exchange will facilitate the development of general predictive models relating trace metal concentrations in insects to those in their environment. Such models will facilitate the use of insects as contaminant biomonitors.