TLC—HPLC法测定小活络丸内中乌头碱,次乌头碱和乌头碱的含量

采用ＴＬＣ－ＨＰＬＣ法测定小活络丸内中乌头碱、次乌头碱和乌头碱的含量，在硅胶Ｇ薄层板上以石油醚－正己烷－醋酸乙酯－无水乙醇－浓氨水（１：２：５：５：０．５）为展开剂，分离提取酯型三，用Ｒｅｓｏｌｖｅ Ｓｐｈｅｒｉｃａｌ Ｓｉｌｉｃａ柱，以无水乙醇－０．４％醋酸铵水溶液（９７：３）为流动相进行测定，检测波长２３１ｎｍ，平均回收率：８３．２％（中乌头碱）、９２．１（次乌头碱）、８４．１％（乌头碱）。     

TLC一HPLC法测定小活络丸内中乌头碱、次乌头碱和乌头碱的含量

采用ＴＬＣ－ＨＰＬＣ法测定小活络丸内中乌头碱、次乌头碱和乌头碱的含量。在硅胶Ｇ薄层板上以石油醚（６０～９０℃）－正己烷－醋酸乙酯－无水乙醇－浓氨水（１：２：５：５：０．５）为展开剂，分离提取酯型生物碱，用Ｒｅｓｏｌｖｅ　Ｓｐｈｅｒｉｃａｌ　Ｓｉｌｉｃａ柱（５μｍ，１５０ｍｍ×３．９ｍｍ），以无水乙醇－０．４％醋酸铵水溶液（９７：３）为流动相进行测定，检测波长２３１ｎｍ，平均回收率：８３．２％（中乌头碱）、９２．１（次乌头碱）、８４．１％（乌头碱）。     

肾康片质量标准的研究

目的：研究肾康片的质量标准并控制该制剂的质量。方法：用薄层色谱法鉴别了肾康片中的黄芪,山茱萸,桑寄生及丹参,用薄层色谱法限量检查屯该制剂中的乌头碱,用双波长薄层扫描法测定了该制剂中黄芪甲苷的含量。结果：乌头碱限量符合中国药典测定,黄芪甲苷的平均回收率为９７．５％,其ＲＳＤ为１．４３％。结论：本文的结果显示出这些方法可用于控制该制剂的质量,方法灵敏,简便,专属,准确。     

高效液相色谱法测定肤得乐凝胶剂中次乌头碱的含量

目的 建立肤得乐凝胶剂中次乌头碱的含量测定方法。方法 采用高效液相色谱法测定次乌头碱的含量，色谱柱为ODS柱；流动相为甲醇-0．1％三乙胺（80：20）；检测波长230nm。结果 次乌头碱在0．224～1．12μg范围内呈良好的线性关系，加样平均回收率为98．34％，RSD为2．30％。结论 本法简单，快速，结果准确，可作为该制剂的质量控制方法。     

中药制剂中乌头碱含量的测定及其临床应用

目的：建立乌头碱中毒的临床和法医学检验的检测方法。方法：结合乌头碱中毒的临床症状，采用高效液相色谱法检测中毒者所服药品中乌头碱含量，计算出病人服用的乌头碱量是否达到中毒量和致死量，从而为临床诊断乌头碱中毒提供检测方法和量化依据。结果：测定的线性范围为1．8－7．3μg，回收率和RSD为97．87％，1．85％。结论：本方法简便、快速、准确，可为乌头碱药酒中毒的临床诊断和法医鉴定提供检测依据。     

吴茱萸汤不同配伍情况下生物碱含量的RP—HPLC测定

目的：采用反相高效液相色谱法测定吴茱萸汤不同配伍情况下的各处方中吴茱萸碱和吴茱萸次碱的含量。方法：ＯＤＳ柱,以乙腈－水－四氢呋喃－冰醋酸（４８：５２：１：０．１）为流动相,氯氟舒松为内标,紫外检测波长２２５ｎｍ。结果：吴茱萸单味药中吴茱萸碱和吴茱萸次碱的回收率分别为９７．１％、９３．７％;ＲＳＤ分别为２．５％,２．６％ｎ＝。结论：本方法操作简单,准确,易行。     

壳聚糖-恶丙嗪缓释片的研制

目的：研究壳聚糖－恶丙嗪缓释片的制备、质量标准,并考察体外释药性能。方法：采用紫外分光光度法测定主药恶丙嗪的含量。结果：线性范围为２．５～１５．０ｕｇ／ｍｌ,平均回收率为９９．７９％,ＲＳＤ为０．３８％。结论：该制剂制备工艺简单,值得临床推广应用。     

薄层扫描法测定消解灵冲剂中马来酸氯苯那敏含量

目的：建立消解灵冲剂中马来酸氯苯那敏含量测定方法，并对其进行评价。方法：样品氯仿提取液经硅胶ＧＦ２５４薄层层析，以乙酸乙酯－甲醇－稀醋酸（５∶３∶２）为展开剂，单波长反射法线性扫描测定氯苯那敏斑点面积，λ＝２６４ｎｍ。结果：标准曲线范围１～５μｇ，平均回收率为９８．２％（ＲＳＤ＝３．５０％），样品中其它成分对本法不存在干扰。结论：本法简便、准确，可用于该制剂的含量测定     

高效液相色谱法与凝胶层析法检测人血白蛋白制剂中多聚体的…

对１２批人血白蛋白制剂分别以ＨＰＬＣ法重复测定５次及用凝胶层析法重复测定４次。结果表明：ＨＰＬＣ法（ＲＳＤ０．２３％－２．８６％）较凝胶层析法（ＲＳＤ１．４１％－５．７０％）结果准确；ＨＰＬＣ法样品不稀释，直接进样，每样仅需３０ｍｉｎ，操作简便易行，可作为白蛋白制剂中多聚体的含量测定方法。     

二阶导数分光光度法测定复方美沙芬洛芬含量

目的：测定复方美沙芬布洛芬含量。方法：以甲醇为溶剂,采用二阶导数分光光度法,用峰－谷法测定,美沙芬、布洛芬的测定波长分别为２９２．３ｎｍ、２８８．２ｎｍ、２６３．８ｎｍ。结果：美沙芬在３．０７－１５．３５μｇ／ｍｌ,布洛芬在３９．８８－１９９．４０μｇ／ｍｌ范围内呈线性关系,其平均回收率分别为９８．２％和９８．７％,ＲＳＤ皆为０．４％－０．７％。结论：本法快速、准确,适应合于该制剂的含量测定。     

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.     

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.