HPLC测定皮肤病血毒丸中大黄素与大黄酚含量

目的:用HPLC测定皮肤病血毒丸中大黄素与大黄酚含量。方法:色谱柱:C18色谱柱,流动相:甲醇-0．1％磷酸溶液(22:78),检测波长430 nm。结果:大黄素在0．01-0．1 μg,大黄酚在0．02～0．12 μg范围内呈良好的线性关系。平均回收率大黄素为98．8％(RSD=1．2％),大黄酚为99．0％(RSD=1．4％)。结论:该方法准确可靠。     

HPLC法测定麻仁丸中大黄素和大黄酚的含量

目的:建立麻仁丸中大黄素和大黄酚含量测定的方法。方法:色谱柱为Thermo ODS C18柱(250 mm×4．6 mm,5μm),流动相为甲醇-0．1％磷酸溶液(85:15),流速为1．0 ml·min-1,检测波长为254 nm。结果:大黄素在0．01-0．29μg(r =0.999 5);大黄酚在0．03-0．52μg(r=0．999 4)范围内线性关系良好。大黄素及大黄酚的平均回收率分别为100.4％(RSD =0．9,n=5),100．1％(RSD=0．3％,n=5)。结论:方法准确可靠。     

HPLC测定复方胆通胶囊中大黄素和大黄酚的含量

目的:建立以高效液相色谱法测定复方胆通胶囊中大黄素和大黄酚含量的方法。方法:色谱柱为C18柱(250 mm×4．6 mm,5μm),流动相为乙腈-水(85:15);检测波长254 nm;流速为0．8 mL·min-1。结果:大黄素和大黄酚在0．01～0．06 mg和0．02～0．12 mg范围内呈良好的线性关系;相关系敬分别0．999 0和0．999 2;大黄素和大黄酚的平均加样回收率专99．12％(RSD=1．2％)和99．52％(RSD=0．6％)。结论:该方法灵敏、简便,结果准确,适用于复方胆通胶囊中大黄素、大黄酚含量测定。     

高效液相色谱法测定妇科消炎0号颗粒剂中大黄素和大黄酚的含量

目的:建立妇科消炎0号颗粒剂中大黄素和大黄酚含量测定的方法。方法:采用高效液相色谱法,色谱柱为Hypersil ODS2柱(250 mm×4．6 mm,5μm),流动相为甲醇-0．1％磷酸(83:17),波长为254 nm。结果:大黄素的线性范围为0．04～0．45μg,r=0．999 9;大黄酚的线性范围为0．04～0．48μg,r=0．999 9;大黄素和大黄酚的平均加样回收率分别为100．21％～101．45％,95．50％～95．95％,RSD分别为0．18％～1．2％,0．18％～0．70％(n=3)。结论:用高效液相色谱法测定妇科消炎0号颗粒剂中大黄素和大黄酚含量,方法准确、简便易行。     

高效液相色谱法测定上清丸中大黄素和大黄酚的含量

目的建立上清九中大黄素和大黄酚的含量测定方法。方法色谱柱为Diamonsil C18（250mm×4．6mm,5μm）,流动相为甲醇-0．1％磷酸溶液（85：15）,流速：1．OmL·min^-1,检测波长：254nrn。结果大黄素进样量在0．0576～0．1536μg线性关系良好,r=0．9999,平均加样回收率为98．49％,RSD为1．75％（n=6）;大黄酚进样量在0．1397～0．3725μg线性关系良好,r=0．9998,平均加样回收率为98．86％,RSD为1．24％（n=6）。结论该方法操作简便,结果准确,重现性好,适用于上清丸中大黄素和大黄酚的含量测定。     

HPLC法测定脑塞安胶囊中大黄素和大黄酚含量

目的用HPLC方法测定脑塞安胶囊中大黄素和大黄酚的总含量。方法采用外标法以甲醇-0．1％磷酸（85：15）为流动相,检测波长为254nm,流速为1．0mL／min。结果大黄素和大黄酚分别在0．2～6．4μg／mL（r=1．0000）和0．8—25．6μg/mL（r=0．9994）范嗣内呈良好的线性,大黄素与大黄酚总平均回收率为96．9％,其RSD值为0．5％（n=9）。结论本法简便、准确、灵敏、重复性良好,适用于脑塞安胶囊的质量控制。     

高效液相色谱法测定痔疮胶囊中大黄素和大黄酚的含量

目的：建立高效液相色谱法测定痔疮胶囊中大黄素和大黄酚含量的方法。方法：采用C18柱（250mm×4．6mm,5μm）,以甲醇-0．1％磷酸液（75：25）为流动相,流速为1．0ml·min^-1,检测波长为254nm。结果：痔疮胶囊中大黄素和大黄酚能有效分离,且无杂质干扰。大黄素在0．0261—0．1480μg（r=0．9999）、大黄酚在0．0509—0．2886μg（r=0．9998）均呈良好线性关系。大黄素和大黄酚平均回收率分别为99．0％和98．8％,（n=9,RSD均为1．3％）。结论：本法简便、快速、准确、可靠。     

不同厂家大黄碳酸氢钠片中大黄素、大黄酚的含量考察

目的考察8个厂家大黄碳酸氢钠片中大黄素、大黄酚的含量。方法采用高效液相色谱法,色谱柱为C18（250mm×4．60mm,5μm）,流动相为甲醇-0．1％磷酸溶液（85：15）,检测波长为254nm,柱温为35℃,流速为1．0ml／min。结果方法线性关系良好,大黄素、大黄酚含量测定的平均回收率分别为96．67％、99．90％,RSD分别为0．57％、0．84％。测定8个厂家生产的15批大黄碳酸氢钠片,结果样品中大黄素和大黄酚含量具有显著性差异。结论大黄碳酸氢钠片的现行标准不能有效控制产品质量,采用HPLC法测定大黄碳酸氢钠片中大黄素和大黄酚的含量,方法简便、准确、重现性好,可以作为大黄碳酸氢钠片的质量控制方法。     

清热暗疮片中大黄素与大黄酚的含量测定

目的：建立清热暗疮片中大黄素与大黄酚的含量测定方法。方法：采用HPLC法进行含量测定，以十八烷基硅烷键合硅胶为填充剂，甲醇-0．1％磷酸溶液（85：15）为流动相，检测波长254nm，流速为1．0ml·min^-1.结果：大黄素在0．0112～0．0560μg，大黄酚在0．0224～0．1120μg范围内峰面积与进样量有良好的线性关系。大黄素的平均回收率为98．6％，RSD为1．17％，大黄酚的平均回收率为98．9％，RSD为1．02％。结论：所建立的方法可以有效地控制制剂的质量。可准确、快速地进行定性、定量检测。     

HPLC法测定胆石通片中大黄素和大黄酚的含量

目的：建立高效液相色谱法同时测定胆石通片中大黄素、大黄酚含量的方法。方法：采用Waters C18色谱柱（250mm×4．6mm,5μm）;流动相：乙腈-水-冰醋酸（60：40：1）;流速：1．0ml·min^-1;检测波长：254nm。结果：大黄素、大黄酚分别在34．56～345．60ng和78．4～784．0ng的范围内呈良好的线形关系,相关系数分别为0．9999和0．9995,平均回收率分别为98．6％和97．3％,RSD分别为0．4％和0．7％。结论：该方法简便易行,结果准确,重复性好,可用于胆石通片的质量控制。     

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.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

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.     

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.