腺苷钴胺凝胶中腺苷钴胺的含量测定

目的 采用高效液相色谱(HPLC)法测定腺苷钴胺凝胶中的腺苷钴胺含量. 方法色谱柱为Uitimate Column XB C₁₈(4.6 mm×250 mm,5 μm),以0.05 mol.L^-1磷酸二氢钾溶液(用磷酸调节pH为3.2)-乙腈(83:17)为流动相;柱温:35 ℃;进样量:10 μL;流速:1.0 mL.min^-1,检测波长:260 nm. 结果 腺苷钴胺在10～50 μg.mL^-1范围内线性关系良好(r＝0.999 9),平均回收率为99.49%,RSD为0.60%(n＝9). 结论 该方法专属性强、准确,可用于测定腺苷钴胺凝胶的含量.     

高效液相色谱法测定天宁颗粒中阿魏酸含量

目的 建立测定天宁颗粒中阿魏酸的高效液相色谱(HPLC)法. 方法 采用反相高效液相色谱法测定阿魏酸的含量. 应用Diamonsil ODS C18色谱柱(200 mm×4.6 mm,5 μm),流动相为乙腈 0.1%磷酸溶液(20：80),检测波长为322 nm,流速：1 mL.min^-1;进样量：20 μL;柱温：室温. 结果阿魏酸浓度在1.0～100.0 μg.mL^-1范围内线性关系良好,r＝0.999 6;平均回收率为 99.78%,RSD＝2.96%(n＝9). 结论 该方法 专属性强,操作简单,结果准确,重复性好,可用于天宁颗粒中阿魏酸的含量测定.     

高效液相色谱法测定氯磺丙脲片的含量

目的 建立高效液相色谱(HPLC)法测定氯磺丙脲片的含量. 方法 岛津 VP-ODS 色谱柱(4.6 mm×250 mm,5 μm);乙腈 磷酸二氢铵溶液(pH3.5)(70:30)为流动相;检测波长207 nm;流速1.0 mL.min^-1;柱温:室温;进样量:20 μL. 结果 氯磺丙脲在20.04～801.60 μg.mL^-1浓度范围内与峰面积呈良好的线性关系(r＝0.999 8);平均回收率为99.65%(n＝9). 结论 该方法定量准确,可用于测定氯磺丙脲片的含量.     

反相高效液相色谱法测定小儿速热清口服液中黄芩苷和连翘苷含量

目的 采用反相高效液相色谱法同时测定小儿速热清口服液黄芩苷、连翘苷的含量. 方法 色谱柱为KromasilC18柱(150 mm×4.6 mm ,5 μm), 流动为甲醇 -水- 0.4%磷酸(40：60：1), 流速为 1.0 mL•min^-1 ,检测波长为 277 nm, 柱温25 ℃. 结果黄芩苷、连翘苷分别在 1.8～18 μg•mL^-1(r＝0.999 8), 0.45～4.50 μg•mL^-1(r＝0.999 6)范围内呈线性关系,加样回收率分别为 99.83% (RSD＝0.26 %),99.78%(RSD ＝0.12%). 结论该方法 操作简便, 结果准确、可靠,同时测定两种成分, 为提高药品质量标准提供参考.     

高效液相色谱法测定维生素B2片的含量

目的 建立高效液相色谱(HPLC)法测定维生素B₂片的含量. 方法 采用Agilent HC-C₁₈(100 mm×4.6 mm,3.5 μm)色谱柱,以乙腈-0.008 mol.L^-1己烷磺酸钠-三乙胺-冰醋酸( 12:87:0.25:0.75)为流动相,流速1.0 mL.min^-1,检测波长267 nm,进样:20 μL,柱温30 ℃. 结果 维生素B2在0.05～0.40 μg范围内线性较好(r＝0.999 9),平均回收率为98.56% (RSD为0.37%). 结论 该方法快速、简便、可靠、准确度高、重复性好,用于维生素B₂片含量测定.     

高效液相色谱法测定头孢克洛分散片的含量

目的 建立高效液相色谱法测定头孢克洛分散片中头孢克洛的含量. 方法色谱柱为资生堂SCX柱(4.6 mm×250 mm,5 μm),流动相为磷酸二氢钾溶液-乙腈(95:5),检测波长为254 nm,流速为1.0 mL•min^-1,柱温:21 ℃. 结果 头孢克洛在0.010 4 ～0.622 3 mg•mL^-1范围内呈良好线性关系,r＝0.999 9(n＝7),平均回收率为100.54%, RSD=1.03%(n＝9). 结论 该方法简便、快速、准确、灵敏度高,可用于头孢克洛的含量测定.     

高效液相色谱法测定鼻通合剂中木兰脂素的含量

目的 建立高效液相色谱(HPLC)法测定鼻通合剂中木兰脂素的含量. 方法 色谱柱为Hypersil BDS柱(4.6 mm×200 mm, 5 μm); 流动相为乙腈-四氢呋喃-水(44：1：55); 流速为1.0 mL•min^-1; 检测波长278 nm; 柱温为30 ℃; 灵敏度为0.10 AUFS. 结果木兰脂素在7.28～232.96 μg•mL^-1浓度范围内线性关系良好, r＝0.999 9, 平均回收率为98.6%(RSD＝1.31%), 97.8%(RSD＝1.25%), 99.5%(RSD＝0.96%). 结论该方法 操作简便, 快捷, 可靠性高, 准确性和重现性好, 其他组分对测定无干扰, 可作为鼻通合剂的质量控制方法 .     

紫草解毒软膏质量标准研究

目的 建立紫草解毒软膏的质量标准. 方法 采用薄层色谱(TLC)法对其中盐酸小檗碱、紫草进行鉴别;高效液相色谱(HPLC)法测定其中左旋紫草素的含量,色谱柱为Hypersil BDS C₁₈柱(4.6 mm×250 mm,5 μm);流动相为甲醇-0.2%磷酸(25：75);流速为1.0 mL.min^-1;检测波长516 nm;柱温为30 ℃. 结果TLC鉴别盐酸小檗碱、紫草具有很好的分离效果. 左旋紫草素在4.47～143.10 μg.mL^-1浓度范围内线性关系良好,r＝0.999 9,平均回收率为97.5%(RSD＝1.42%). 结论 所建立的鉴别方法 专属性强,定量方法 简便,准确,可用于紫草解毒软膏的质量控制.     

高效液相色谱法测定菝葜醋酸乙酯提取物中白藜芦醇的含量

目的建立高效液相色谱法测定菝葜醋酸乙酯提取物中白藜芦醇含量的方法。方法Zirchrom Kromasil C18 色谱柱(4.6 mm×250 mm，5 μm)；流动相：乙腈-水(30∶70)；流速：1.0 mL·min^-1；柱温：室温；检测波长303 nm。结果白藜芦醇对照品线性范围18.8～94.0 μg·mL^-1，r＝0.999 6(n＝5)，样品平均回收率为101.10 %，RSD＝0.64 %(n＝5)，菝葜醋酸乙酯提取物中白藜芦醇的平均含量为29.59 μg·mg^-1。结论该方法简便、快捷、重现性好，为菝葜醋酸乙酯提取物的质量控制提供依据。     

中空纤维分离-高效液相色谱法测定复方痤疮凝胶中主药的含量

目的 建立中空纤维分离-高效液相色谱(HPLC)法测定复方痤疮凝胶剂中主药含量的方法. 方法 采用中空纤维处理凝胶样品,含量测定以Venusil XBP-C₁₈色谱柱(4.6 mm×150 mm,5 μm)为固定相,以磷酸盐缓冲液(取0.015 mol.L^-1磷酸二氢钾溶液,磷酸溶液调节pH至3.0)-乙腈为流动相进行梯度洗脱;进样量:20 μL;柱温:30 ℃;流速:1.0 mL.min^-1;紫外检测波长:克林霉素磷酸酯:210 nm,维A酸:350 nm. 结果 主成分峰与相邻杂质峰分离度＞1.5. 克林霉素磷酸酯在48.00～480.00 μg.mL^-1范围内线性关系良好,r＝0.999 8,平均回收率为99.96%,RSD为0.69%(n＝6),维A酸在1.00～20.00 μg.mL^-1范围内线性关系良好,r＝0.999 7,平均回收率为99.99%,RSD为1.24%(n＝6). 结论 该方法简单、可靠,可用于复方痤疮凝胶剂中的样品处理和含量测定.     

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.