高效液相色谱法测定复方丹参片和滴丸中丹酚酸B和丹参酮ⅡA的含量

目的:测定复方丹参片和复方丹参滴丸中丹酚酸B和丹参酮ⅡA的含量,比较两种丹参制剂的内在质量区别.方法:采用高效液相色谱(HPLC)方法测定丹酚酸B和丹参酮ⅡA在两种制剂中的含量.结果:复方丹参片中丹酚酸B和丹参酮ⅡA的含量比复方丹参滴丸中的含量高.结论:两种丹参制剂的内在质量差别很大.     

校正因子在阿莫西林/克拉维酸钾片含量测定中的应用探讨

目的 在阿莫西林/克拉维酸钾片中,利用阿莫西林对照品对克拉维酸进行含量测定.方法 计算克拉维酸与阿莫西林之间的校正因子,用阿莫西林对照品加校正因子对克拉维酸的含量进行测定.结果阿莫两林与克拉维酸进样量分别在0.2178～6.5340μg(r=1.0000)与0.0632～1.897μg(r=1.0000)范围内与其峰面积呈良好的线性关系,克拉维酸与阿莫西林之间的校正因子f=1.330,克拉维酸回收率为99.29%(n=9).结论 将校正凶子应用到阿莫西林克拉维酸钾片中进行含量测定是可行的、实用的.     

高效液相色谱法测定复方丹参片和滴丸中丹酚酸B和丹参酮IIA的含量

目的：测定复方丹参片和复方丹参滴丸中丹酚酸B和丹参酮IIA的含量，比较两种丹参制剂的内在质量区别。方法：采用高效液相色谱(HPLC)方法测定丹酚酸B和丹参酮IIA在两种制剂中的含量。结果：复方丹参片中丹酚酸B和丹参酮IIA的含量比复方丹参滴丸中的含量高。结论：两种丹参制剂的内在质量差别很大。     

复方丹参片与滴丸中丹酚酸B和丹参酮Ⅱ_A含量的比较研究

目的:测定并比较复方丹参片与滴丸中丹酚酸B和丹参酮ⅡA的含量。方法:色谱柱为EclipseXDBC18,丹酚酸B、丹参酮ⅡA流动相分别为甲醇-0·2%磷酸溶液(40∶60)、甲醇-水(85∶15),流速为1·0ml/min,柱温为30℃,检测波长为280nm。结果:丹酚酸B和丹参酮ⅡA进样量均在0·1μg~2·0μg范围内与峰面积值呈良好线性关系(r丹酚酸B=0·9998、r丹参酮ⅡA=0·9999);复方丹参片中丹酚酸B、丹参酮ⅡA的平均回收率分别为100·7%(RSD=1·9%)、101·0%(RSD=1·5%),复方丹参滴丸中丹酚酸B、丹参酮ⅡA的平均回收率分别为98·6%(RSD=1·2%)、98·8%(RSD=1·4%)。结论:本方法准确、可靠、重现性好;复方丹参片中丹酚酸B和丹参酮ⅡA含量较高,复方丹参滴丸中则未定量检出上述2成分。     

HPLC法同时测定复方丹参口服液中羟基红花黄色素A和丹酚酸B的含量

目的:建立同时测定复方丹参口服液中羟基红花黄色素A和丹酚酸B含量的方法。方法:采用高效液相色谱法。色谱柱为SHIMADZU ODS-C18,流动相为甲醇-0.5%磷酸(35∶65,V/V),流速为1.0 ml/min,检测波长为403 nm(羟基红花黄色素A)、286nm(丹酚酸B),柱温为35℃,进样量为20μl。结果:羟基红花黄色素A、丹酚酸B检测质量浓度线性范围分别为2.01~20.10、39.80~398.00μg/ml(r均为0.999 9);精密度、稳定性、重复性试验的RSD<2%;加样回收率分别为98.26%~101.25%、98.70%~101.35%,RSD分别为0.94%、0.71%(n=9)。结论:该方法简便可行、重复性好,可用于复方丹参口服液中羟基红花黄色素A和丹酚酸B的含量测定。     

丹参注射剂中丹参素、原儿茶酸、原儿茶醛和丹酚酸B的同时测定

目的:建立高效液相色谱法测定丹参注射剂中丹参素、原儿茶酸、原儿茶醛和丹酚酸B等4种有效成分的含量。方法:色谱柱为Hypersil C18(4.6 mm ×250 mm,5μm);流动相由甲醇(A)和5％冰醋酸(B)组成,进行梯度洗脱,在0～5 min,B体积分数为90％,5～10 min,B体积分数由90％线性改变至65％,10～20 min,维持B体积分数为65％,流速为1.0 mL·min-1;柱温30℃,检测波长为281 nm;对羟基苯甲酸作为内标物。结果:丹参素、原儿茶酸、原儿茶醛和丹酚酸B浓度分别在3.95～47.4μg·mL-1(r=0.9996)、4.47～53.6μg·mL-1(r=0.9996)、5.14～61.7μg·mL-1(r=0.9999)和8.40～117μg·mL-1(r=0.9994)范围内呈良好线性关系,丹参素、原儿茶酸、原儿茶醛、丹酚酸B的平均回收率分别为99.45％(RSD=3.6％,n=6),97.57％(RSD=2.8％,n=6),100.2％(RSD=3.9％,n=6)和100.2％(RSD=3.2％,n=6)。测定了6批丹参注射液样品。结论:方法简便,分离效果好,能同时测定丹参注射剂中丹酚酸B、丹参素、原儿茶醛、原儿茶酸等4种水溶性成分的含量,结果准确可靠。     

HPLC法测定妇炎舒片中丹酚酸B的含量

目的建立妇炎舒片中丹酚酸B的含量测定方法。方法以丹酚酸B为测定指标,HPLC测定妇炎舒片中丹酚酸B的含量。色谱条件：色谱柱为KromasilC18（250mm×4.6mm,5μm）;流动相：甲醇-乙腈-甲酸-水（30：10：1：59）;检测波长：286nm;流速：1.0mL/min。结果丹酚酸B对照品在0.508～3.176μg范围内线性关系良好,r=0.9999;平均回收率为97.94%,RSD=1.14（n=6）。结论本定量方法简便、准确、专属性强,能有效控制妇炎片的质量。     

超微粉固体分散技术对丹参片指标成分溶出度的影响

目的：采用超微粉固体分散技术制备丹参片,并考察其溶出特征。方法：按《中国药典》2015年版丹参片制备方法制得丹参片DSP1作为对照品,用超微粉固体分散技术制得丹参片DSP2。高效液相色谱（HPLC）法测定2种丹参片中的丹酚酸B、丹参酮Ⅱ_A的含量,并在不同溶出介质测定各成分的溶出度,绘制溶出曲线,采用f₂相似因子法进行比较分析。结果：DSP1、DSP2的丹酚酸B含量分别为11.20,18.90 mg·g^-1原药材,丹参酮Ⅱ_A含量分别为0.45,0.71 mg·g^-1原药材;丹酚酸B、丹参酮Ⅱ_A在0.1 mol·L^-1的盐酸溶液介质中溶出曲线的相似因子分别为40,32,在0.5%十二烷基硫酸钠（SDS）水溶液中溶出曲线的相似因子分别为43,35,f₂<50,两种丹参片的溶出度有显著差异。结论：超微粉固体分散技术能显著高丹参片中的丹酚酸B、丹参酮Ⅱ_A溶出度,同时提高丹参药材的利用率,值得进一步研究推广。     

一测多评法测定丹参-红花药对不同配伍比例中5种成分含量

摘要：目的:建立一测多评法（QAMS）同时测定丹参-红花药对不同配伍比例中羟基红花黄色素A、丹酚酸B、隐丹参酮、丹参酮Ⅰ、丹参酮ⅡA的含量。方法:采用GL Sciences ODS C18（250 mm×4.6 mm, 5μm）色谱柱,流动相为乙腈-0.2%磷酸水溶液,梯度洗脱,流速为1.0 ml·min-1,柱温为30℃。以丹参酮ⅡA为内标物,计算羟基红花黄色素A、丹酚酸B、隐丹参酮、丹参酮Ⅰ的相对校正因子,并测定其含量。结果:羟基红花黄色素A、丹酚酸B、隐丹参酮、丹参酮Ⅰ、丹参酮ⅡA在各自范围内线性关系良好（r＞0.999 0）,平均加样回收率为95.90%～103.45%,RSD为0.50%～2.08%（n=6）。一测多评法计算结果与外标法实测值无明显差异。结论:所建立的一测多评法可用于丹参-红花药对中5种成分含量的同时测定。     

不同生产企业复方丹参片中丹酚酸B的含量测定

目的分析不同企业生产的复方丹参片的质量控制情况.方法采用高效液相色谱法测定丹酚酸B的含量.结果与结论测定结果看出标准提高后各生产企业不仅重视了丹参药材的质量而且很好的控制了生产工艺,提高了水溶性成分丹酚酸B的含量,合格率达到94%,有效的提高了复方丹参片的质量.     

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.