明胶空心胶囊铬元素AAS法测定不确定度评定研究

目的：建立原子吸收法测定明胶空心胶囊中铬元素不确定度评定的方法。方法：采用《中国药典》2015年版收载明胶空心胶囊铬元素测定的方法,找出影响测定结果的各个分量并量化各组成标准不确定度,评定测定结果的不确定度。结果：原子吸收测定明胶空心胶囊铬元素的不确定度为1.395±0.08487 μg·mL^-1（k=2）。结论：本方法简便易行,可用于原子吸收法测定明胶空心胶囊中铬元素的不确定度评定。     

明胶空心胶囊中7种元素含量测定方法的建立与应用

目的:为明胶空心胶囊质量的提高提供参考。方法:采用原子荧光光度法测定明胶空心胶囊中汞、砷的含量,石墨炉原子吸收法测定铬、铅和镉的含量,火焰原子吸收法测定铜和锌的含量,并对48批市售明胶空心胶囊的7种元素含量进行测定。结果:各元素在各自的检测质量浓度范围内(铬、铅、镉、砷、汞分别为0~10、0~20、0~1.5、0~10、0~1.0μg/L,铜、锌均为0~1.8 mg/L)线性关系良好(r≥0.996 9);铬、铅、镉、铜、锌、汞、砷检测限分别为0.065、0.007、0.011、0.004、0.010、0.108、0.004μg/L;精密度试验的RSD均不大于2.5%(n=6);重复性试验的RSD均不大于7.5%(n=6);平均加样回收率在88.6%~109.5%之间,RSD均不大于6.7%(n=6)。48批市售样品中7种元素含量均符合2015年版《中国药典》(四部)及其他国家或组织药典或标准中的相关规定。结论:本方法灵敏度与精密度高、结果准确可靠,可用于明胶空心胶囊中铬、铅、镉、铜、锌、汞、砷7种元素的含量测定;不同厂家生产的48批明胶空心胶囊质量情况较好。     

人工养殖赤子爱胜蚓中重金属及有害元素的测定

目的 建立人工养殖赤子爱胜蚓中铅、镉、砷、汞、铜含量测定的方法,并测定6批赤子爱胜蚓药材中铅、镉、砷、汞、铜的含量。方法 采用微波消解样品,用石墨炉原子吸收法测定铅、镉的含量;火焰原子吸收法测定铜的含量;原子荧光光谱法测定砷、汞含量。结果 铅的回收率为103.6%（RSD=6.4%）,镉的回收率在92.0%（RSD=7.7%）,铜的回收率在101.6%（RSD=8.1%）,砷的回收率在94.4%（RSD=4.7%）,汞的回收率在93.6%（RSD=5.4%）。结论 本方法操作简便、快速,且准确度和精密度高,适合于赤子爱胜蚓药材中铅、镉、铜、汞和砷的含量测定。     

中药粉碎前后重金属铬含量检测分析

摘 要 目的： 通过对多批次样品（包括中药材、中药饮片、中成药、药用辅料）粉碎前后的铬含量检测,证明通过不锈钢材质制药机械进行中药细粉加工将导致产品重金属铬超标。方法: 参照《中国药典》2010年版一部附录Ⅸ B铅、镉、砷、汞、铜测定法,参考《中国药典》2010年版二部明胶空心胶囊“铬”[检查]标准。结果: 大部分检验数据显示,样品的铬含量不同程度超标。结论:使用不锈钢材质的制药机械设备会导致中药生产过程中铬超标,给产品质量带来安全隐患。     

水蛭中重金属元素的含量测定及分析

摘 要 目的：测定25批次不同生产企业的水蛭药材中铅、镉、砷、汞、铜和铬的含量并进行分析。方法: 微波消解法处理样品,然后采用电感耦合等离子质谱法测定25批次水蛭药材中铅、镉、砷、汞、铜和铬的含量并运用SPSS16.0软件对数据进行聚类分析。结果: 25批次水蛭药材中,砷、汞、铜和铬均有不同程度超出规定限度, 铅和镉均符合现行标准。结论: 分析了不同生产企业水蛭中重金属含量差异特点及超标的可能原因,为水蛭药材的规范化养殖,安全评价及重金属含量标准制定提供一定依据。     

湿法消解-AAS法测定明胶空心胶囊中铬的含量

目的：建立原子吸收分光光度（ AAS）法测定明胶空心胶囊中铬的含量。方法样品湿法消解处理后,采用AAS法测定明胶空心胶囊中铬的含量。结果铬在5～80ng· mL －1范围内线性关系良好,相关系数为0.9991;平均回收率为100.8％（n＝6）,RSD为5.8％。结论本方法简单、快速、准确;可用于明胶空心胶囊中有害重金属铬的质量控制。     

原子吸收分光光度法测定薄膜包衣预混剂中的铅、铁含量

摘 要 目的： 建立原子吸收分光光度法测定薄膜包衣预混剂中铅、铁含量的分析方法。方法: 样品经微波消解,采用石墨炉法测定铅含量,火焰法测定铁含量。结果: 铅质量浓度在1.0～5.0 μg·L^-1范围内与吸光度线性关系良好（r=0.999 4）;铁质量浓度在0.1～1.0 mg·L^-1范围内线性关系良好（r=0.998 4）。铅的回收率为91.3%（RSD=1.4%,n=9）;铁的回收率为89.9%（RSD=3.5%,n=9）。结论:该方法准确、稳定,可较好地用于薄膜包衣预混剂铅、铁的含量测定。     

ICP-MS测定明胶空心胶囊中铅、铬、镉、砷、铜的含量

目的建立明胶空心胶囊中有害重金属元素含量的测定方法,对空心胶囊质量进行控制。方法采用HN03对明胶空心胶囊进行微波消解制样,利用电感耦合等离子体质谱法（ICP-MS）同时测定样品中5种重金属元素铅、铬、镉、砷、铜的含量。结果部分被测样品中铅、铬、砷有超标现象。该方法的加样回收率为95．4％-104．6％,RSD为1．8％-3．0％。结论本方法操作简便、结果可靠,可用于明胶空心胶囊中重金属元素含量的测定。     

明胶空心胶囊中铬含量测定方法研究进展

目的:为加强明胶空心胶囊的质量控制提供参考。方法:通过查阅近5年国内外相关文献资料,对明胶空心胶囊中铬含量测定方法的研究进展进行综述。结果:明胶空心胶囊中铬含量测定方法主要有原子吸收分光光度(AAS)法、分光光度(UV)法、X射线荧光分析(XRFA)法和电感耦合等离子体质谱(ICP-MS)法;采用石墨炉原子吸收分光光度(GF-AAS)法时样品的消解方法主要有微波消解法、炉内消解法和高压消解法等。结论:GF-AAS是测定明胶空心胶囊中铬含量的法定方法,UV、XRFA和ICP-MS可以作为其补充。其中ICP-MS作为一种新的检测方法,不仅可以测定明胶空心胶囊中的铬含量,还可以同时测定胶囊壳中其他多种有毒有害元素的含量和进行价态分析,应用前景广阔。     

原子吸收分光光度法测定明胶空心胶囊中铬的不确定度分析

目的分析原子吸收分光光度法测定明胶空心胶囊中铬的不确定度,明确影响不确定度的因素。方法建立原子吸收分光光度法测定明胶空心胶囊中铬的数学模型,确定影响不确定度的因素,并根据《测量不确定度评定与表示》（JJF1059 1999）中有关规定,量化各不确定度分量,计算合成不确定度,从而得出测定结果的扩展不确定度。结果测定结果合成不确定度为0.05 μg•g－1,扩展不确定度为0.10 μg•g－1,明胶空心胶囊中铬的含量为 （1.65±0.10） μg•g－1（K＝2）。结论测定结果不确定度主要来源于供试液中铬浓度的测定影响,因此,原子吸收分光光度仪的稳定性是测量准确与否的关键。所建立的不确定度评估方法适用于原子吸收分光光度法测定明胶空心胶囊中铬含量的不确定度分析。     

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.     

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.     

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.