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-MS法测定依地酸二钠中8种金属元素含量

摘 要 目的：建立ICP MS法测定依地酸二钠中Fe、Ni、Cu、As、Cr、Cd、Hg、Pb等8种金属元素含量。方法: 采用ICP–MS法进行测定,应用碰撞池技术(CCT),最大程度的减少多原子干扰,通过在线加入Sc、Rh、Tb、Lu、Bi 等内标元素的方法,校正测量结果,降低基体效应和信号漂移干扰。样品用纯水溶解成0.1%水溶液,直接进样。结果: 检测限范围为0.009～0.11 ng·ml-1时 ,标准曲线线性关系良好(r在0.997 0～1.000 0范围内）;回收率均在82%～98% 之内(n=6)。结论: 上述方法简便、快速、准确,可用于依地酸二钠中8种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。     

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。     

HPLC-MS/MS法同时测定百蕊颗粒中紫云英苷和山奈酚的含

摘 要 目的：建立同时测定百蕊颗粒中紫云英苷和山奈酚2种有效成分含量的HPLC MS/MS检测方法。方法: 采用Ultimate XB C18 （100 mm×2.1 mm,5 μm）色谱柱;流动相为0.1%甲酸水溶液（A） 0.1%甲酸乙腈(B),梯度洗脱,流速0.3 ml·min-1;柱温为40℃;采用电喷雾离子源(ESI),以多反应监测方式(MRM)进行定量分析。紫云英苷和山奈酚在负离子模式下定量分析离子对分别为m/z 447.2→m/z 284.0和m/z 285.1→m/z 187.1。结果:紫云英苷和山奈酚的浓度分别在9.86~1 970 ng·ml-1（r=0.999 5）和8.73~437 ng·ml-1（r=0.999 6）范围内均呈良好线性关系;紫云英苷和山奈酚低、中、高平均加样回收率分别为99.23%、99.65%、99.23%和98.24%、99.13%、99.69%,RSD分别为1.84%、1.37%、1.21%和1.38%、0.96%、1.47%（n=6）。结论:本文方法简便可靠,重复性好,可同时测定百蕊颗粒中紫云英苷和山奈酚的含量,适用于百蕊颗粒质量控制。     

HPLC法同时测定抗支糖浆中盐酸麻黄碱和苦杏仁苷的含量

摘 要 目的：建立一种HPLC法同时测定抗支糖浆中盐酸麻黄碱和苦杏仁苷含量。方法: 采用Waters ODS2（250 mm×4.6 mm,5 μm）色谱柱,乙腈 0.2%磷酸水溶液（含0.1%三乙胺）梯度洗脱,检测波长为205 nm,流速为1.0 ml·min-1,柱温为30℃。结果:盐酸麻黄碱和苦杏仁苷分别在0.169~3.380 μg（r=0.999 9）、0.141~2.820 μg（r=0.999 7）线性范围良好;平均加样回收率分别为98.8%、99.1%,RSD分别为1.93%、1.22%（n=6)。结论:本方法可同时测定抗支糖浆中盐酸麻黄碱和苦杏仁苷的含量,方法简单准确,重复性好,可用于该制剂的质量控制。     

UPLC-MS/MS法测定黄杨宁制剂中的环维黄杨星D的含量

摘 要 目的：建立超高效液相色谱 串联质谱法（UPLC MS/MS）快速测定黄杨宁制剂中环维黄杨星D的含量。方法: 采用UPLC MS/MS法。色谱柱为Waters ACQUITY UPLC BEH C18柱（100 mm×2.1 mm,1.7 μm）,流动相为乙腈 含0.1%甲酸的0.01 mol·L-1甲酸氨溶液,梯度洗脱,流速为0.35 ml·min-1,柱温为30℃,进样量为5 μl。离子源为电喷雾（ESI）离子源,正离子模式,工作模式为多反应监测模式（MRM）。结果:环维黄杨星D的线性范围为15.58～1 558.00 ng·ml-1（r=0.999 5）;平均加样回收率为97.7%（RSD=3.8%,n=6）。结论:该方法快速、简便、准确、重复性好,适用于黄杨宁制剂的质量控制。     

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。     

湖州市第一人民医院药剂科 浙江湖州 313000

摘 要 目的：建立HPLC法同时测定复方羚角降压片中8种活性成分的含量。 方法: 采用HPLC波长切换法,色谱柱为Agilent ZORBAX Eclipse XDB C18(250 mm×4.6 mm,5 μm),流动相为甲醇(A) 0.06%磷酸溶液(B),梯度洗脱,流速为1.0 ml·min-1,检测波长为265 nm（紫丁香苷）、330 nm（咖啡酸、异迷迭香酸苷、迷迭香酸）、278 nm（黄芩苷、汉黄芩苷、黄芩素、汉黄芩素）,柱温为30℃,进样量为10 μl。 结果: 紫丁香苷、咖啡酸、异迷迭香酸苷、迷迭香酸、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素分别在11.616～69.696 μg·ml-1,1.601～9.605 μg·ml-1,2.040～12.240 μg·ml-1,14.888～89.328 μg·ml-1,72.032～432.192 μg·ml-1,24.016～144.096 μg·ml-1,10.040～60.240 μg·ml-1,1.801～10.805 μg·ml-1(r为0.999 4～0.999 9）浓度范围内呈良好的线性关系;平均加样回收率分别为98.8%,99.7%,98.8%,98.0%,99.1%,99.3%,100.2%,97.4%,RSD分别为0.7%,0.7%,0.4%,0.6%,0.3%,0.5%,0.5%,0.7%（n=6）。 结论: 该方法简单、有效、准确,可用于复方羚角降压片中上述8种活性成分含量的同时测定。     

超高效液相色谱-串联质谱法测定化妆品中地塞米松含量的不确定度分析

摘 要 目的：采用超高效液相色谱 串联质谱法(UPLC MS/MS)对化妆品中地塞米松含量进行测定不确定度评定。方法: 对化妆品中地塞米松含量测定过程中各影响因素包括称量、标准溶液配制、标准曲线拟合、提取过程和仪器测定等进行分析评定。结果:该方法检测化妆品中地塞米松的合成不确定度为0.75 μg·g-1,扩展不确定度为1.5 μg·g-1。本试验测定的化妆品中地塞米松含量结果为(20.4±1.5) μg·g-1（k=2,置信区间p=95%）。结论:评定结果表明,本试验的不确定度主要由标准溶液配制和标准曲线拟合等引入。     

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.

     

In vitro studies on sterically stabilized liposomes (SL) as enzyme carriers in organophosphorus (OP) antagonism

This study describes a new approach for organophosphorous (OP) antidotal treatment by encapsulating an OP hydrolyzing enzyme, OPA anhydrolase (OPAA), within sterically stabilized liposomes. The recombinant OPAA enzyme was derived from Alteromonas strain JD6. It has broad substrate specificity to a wide range of OP compounds: DFP and the nerve agents, soman and sarin. Liposomes encapsulating OPAA (SL)* were made by mechanical dispersion method. Hydrolysis of DFP by (SL)* was measured by following an increase of fluoride ion concentration using a fluoride ion selective electrode. OPAA entrapped in the carrier liposomes rapidly hydrolyze DFP, with the rate of DFP hydrolysis directly proportional to the amount of (SL)* added to the solution. Liposomal carriers containing no enzyme did not hydrolyze DFP. The reaction was linear and the rate of hydrolysis was first order in the substrate. This enzyme carrier system serves as a biodegradable protective environment for the recombinant OP-metabolizing enzyme, OPAA, resulting in prolongation of enzymatic concentration in the body. These studies suggest that the protection of OP intoxication can be strikingly enhanced by adding OPAA encapsulated within (SL)* to pralidoxime and atropine.     

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.     

Alzheimer’s disease – current trends in basic and clinical research. Highlights from the 16th ECNP

Advances in the molecular biological knowledge of neuronal nicotinic acetylcholine receptors (nAChRs) have led to a growing interest by the pharmaceutical industry in the development of novel compounds that selectively modulate nAChR function. The ability of (-)-nicotine, an activator of nAChRs, to enhance attentional aspects of cognition in animals and humans, to exert neuroprotective and anxiolytic-like effects, and presumably to mediate the negative correlation between smoking and Alzheimer's (and Parkinson's) Disease, has focused interest on the potential therapeutic utility of modulators of nAChR function for treatment of some of the deficits associated with these progressive, neurodegenerative conditions. Numerous compounds are known which activate nAChRs and which might serve as lead compounds toward the development of such agents. The pharmacologic diversity of neuronal nAChR subtypes suggests the possibility of developing selective compounds which would have more favourable side-effect profiles than existing agents. This broader class of agents, collectively called cholinergic channel modulators (ChCMs), is anticipated to encompass compounds which would have more favourable side-effect profiles than existing agents, which generally exhibit low selectivity. This selectivity may be achieved by preferentially activating some subtypes of nAChRs (i.e., Cholinergic Channel Activators, ChCAs) or inhibiting the function of other subtypes (Cholinergic Channel Inhibitors, ChCIs). An overview of the biology of nAChRs and the rationale for the use of ChCMs for the treatment of dementia related to neurodegenerative diseases are presented, followed by a discussion of lead compounds and compounds under consideration for clinical evaluation.     

Steroidal sapogenin contents in some domestic plants

In order to find out the values of the steroid resources for the future use. the compositions and contents of steroidal sapogenins from 13 domestic plants have been investigated. As a result,Dioscorea nipponica, D. quinqueloba andSmilax china were found to have large amount of diosgenin. And pennogenin inTrillium kamtschaticum andParis verticillata, yuccagenin inAllium fistulosum, hecogenin inAgave americana and neochlorogenin inSolanum nigum were appeared to be major steroidal sapogenins.