HPLC法同时测定溃结康微丸中芍药苷和黄芩苷的含量

目的:建立溃结康微丸中芍药苷和黄芩苷的 HPLC 含量测定方法。方法:采用 Kromasil C_(18)柱(250 mm×4.6 mm,5.0μm),0.2%磷酸溶液(A)和乙腈(B)为流动相梯度洗脱,流速:1.0 mL·min~(-1),检测波长:230 nm,柱温为25℃。结果:芍药苷在1.749～17.49μg·mL~(-1)(r=0.9996)、黄芩苷在13.33～133.3μg·mL~(-1)(r=0.9998)范围内呈良好的线性关系,平均回收率(n=6)分别为98.2%和97.4%,RSD 分别为1.5%和1.9%。结论:本法简便、快速、准确,可用于溃结康微丸中芍药苷和黄芩苷的同时测定。     

液-质联用测定益智合剂中芍药苷的含量

目的:建立HPLC-MS/MS法测定益智合剂中芍药苷含量的方法.方法:采用高效液相串联质谱法对益智合剂中痕量的芍药苷进行分析,选用ZORBAX C18柱(2.1mm× 30mm,3.5μm)为色谱柱,流动相为甲醇-5 mmol·L-1甲酸铵(75:25),流速为0.4 mL·min-1,柱温:25℃.质谱条件:电喷雾离子源(ESI),检测方式为多离子反应监测(MRM),负离子模式,用于定量分析的离子为m/z525→449.结果:用外标法定量分析,线性范围为20～5000 μg·L-1,r=0.9999;益智合荆中芍药苷的最低检测限为2μg·L-1;精密度RSD为0.84%;平均加样回收率为96.34%,RSD为2.45%(n=5);测得益智合剂中芍药苷的含量为31.45μg·L-1.结论:本法操作简单、快捷,结果准确可靠,可作为有效检测益智合剂中的痕量成分芍药苷含量的方法.     

HPLC法测定同仁乌鸡白凤丸中芍药苷和丹参素的含量

目的:建立测定同仁乌鸡白凤丸中芍药苷和丹参素含量的方法。方法:采用 C_(18)柱(250mm×4.6 mm,5 μm)测定芍药苷的含量,流动相为甲醇-水(30:70),流速1 mL·min~(-1),检测波长232 nm;采用 C_(18)柱(250 mm×4,6 mm,5μm)测定丹参素的含量,流动相为甲醇-0.5%醋酸(8:92),流速1 mL·min~(-1),检测波长281 nm。结果:芍药苷的线性范围为0.0119～0.0595 mg·mL~(-1)(r=0.9993),平均同收率(n=6)为100.1%(RSD 为2.5%);丹参素的线性范同为0.0248～0.1240 mg·mL~(-1)(r=0.9993),平均回收率(n=6)为95.5%(RSD 为1.6%)。结论:本方法操作简便,结果准确可靠,重复性好,可用于同仁乌鸡白凤丸的质量控制。     

RP-HPLC法测定固经丸中芍药苷的含量

目的:建立HPLC法测定固经丸中芍药苷的含量。方法:ZORBAX SB-C_(18)分析柱(250 mm×4.6 mm,5μm);流动相:甲醇-0.05 mol·L~(-1)磷酸二氢钾溶液-三乙胺(28:72:0.5);检测波长:230 nm;流速:1.0 ml·min~(-1),柱温:40℃。结果:芍药苷在0.44～3.96μg范围内的线性关系良好(r=0.9999),平均加样回收率为99.2%(n=5),RSD 1.2%(n=5)。结论:该方法准确,灵敏度高,重现性好。     

HPLC法测定脑通注射液中芍药苷的含量

目的建立脑通注射液中芍药苷含量测定的HPLC法.方法用Water的C18反相色谱柱(4.6 mm×150mm,5 μm),以甲醇-0.03mol·L-1磷酸二氢钾-5%庚烷磺酸钠(65:30:5)为流动相,流速为1.0 mL·min-1,用二极管阵列检测器检测,检测波长230 nm,柱温30℃.结果方法芍药苷在43.9～219.5μg·mL-1呈良好的线性关系(r=0.999 6),精密度RSD为0.23%(n=7),重现性RSD为1.31%(n=5),芍药苷的平均回收率为99.9%,RSD为0.72%(n=6).结论方法快速、简便,结果准确、可靠,可用于脑通注射液中芍药苷的含量测定.     

RP-HPLC法测定小儿柴桂退热颗粒中芍药苷和黄芩苷的含量

目的建立测定小儿柴桂退热颗粒中芍药苷和黄芩苷含量的方法。方法色谱柱:Agela Venusill C_(18)(250mm×4.6mm,5μm);流动相:乙腈-1mL·L~(-1)磷酸水溶液(18∶82);流速:1.0mL·min~(-1),检测波长:0~12min为230nm,12~18min为277nm;柱温:30℃。结果黄芩苷和芍药苷分别在0.254 0~2.032和0.101 0~0.808 0μg范围内呈良好线性关系,平均回收率分别为99.19%和99.14%(n=6),RSD值分别为0.96%和1.09%。结论该方法操作简便,结果准确,重复性好,可作为小儿柴桂退热颗粒中含量测定的检测方法。     

高效液相色谱法测定祛风消白胶囊中芍药苷的含量

目的 建立高效液相色谱法测定祛风消白胶囊中芍药苷含量的方法.方法 采用Diamonsil C18(5μm,4.6×250mm)色谱柱,流动相为甲醇-0.02mol·L-1磷酸二氢钾(25∶75),检测波长:230nm,流速为1.0mL·min-1;柱温35℃.结果 芍药苷进样量在0.058848μg～1.17696μg范围内线性关系良好(r=0.99999),回收率为99.7%,RSD为0.14%(n=6).结论 本方法操作简便、准确、重复性好,可作为控制祛风消白胶囊中芍药苷含量的有效方法.     

HPLC法测定养阴清肺口服液中芍药苷的含量

目的建立HPLC法测定养阴清肺口服液中芍药苷的含量。方法采用高效液相色谱法。色谱柱:CNW Athena 120A C_(18)柱(150mm×4.6 mm,5μm);流动相:乙腈-1 mL·L~(-1)磷酸(12∶88);流速:1.0 mL·min~(-1);检测波长:230nm;进样量:20μL。结果芍药苷在0.593 75~38μg·mL~(-1)范围内线性关系良好(r=0.999 99),平均回收率为99.74%,RSD为2.21%(n=6)。结论该方法准确、灵敏,专属性强,重复性好,对养阴清肺口服液质量控制标准的提高具有参考意义。     

HPLC法测定肝血瘤康糖浆中芍药苷的含量

目的:建立HPLC法测定肝血瘤康糖浆中芍药苷含量的方法.方法:采用DIONEX C18色谱柱(250 mm×4.6 mm,5 μm),甲醇-0.05mol·L-1磷酸二氢钾溶液(38:62)为流动相,流速:1.0ml·min-1,柱温:30℃,检测波长:230 nm.结果:芍药苷在0.12～5.99μg(r=0.999 8)范围内呈良好的线性关系,平均回收率为100.4%(RSD=0.8%,n=6).结论:本方法灵敏、简便、准确,可用于肝血瘤康糖浆中芍药苷的含量控制.     

不同比例配伍的赤芍-藜芦药对中芍药苷和芍药苷内酯的含量测定

目的考察不同比例赤芍与藜芦配伍后芍药苷和芍药苷内酯的含量变化。方法采用HPLC法测定芍药苷和芍药苷内酯的含量;色谱条件:Inertsil C_(18)柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.1 mL·L~(-1)磷酸水溶液(13∶87);检测波长:230 nm;流速:1.0 mL·min~(-1)。结果芍药苷和芍药苷内酯质量浓度分别在7.03～450.00和1.13～290.00μg·mL~(-1)(r=1.000 0)范围内与峰面积呈良好线性关系,平均回收率分别为97.93%(RSD=1.85%)和97.15%(RSD=1.81%)。结论赤芍与藜芦不同比例配伍后芍药苷和芍药苷内酯含量均比赤芍单煎液低,存在减效现象,赤芍-藜芦药对可能为相反配伍。     

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.