HPLC法测定乌藤镇痛胶囊中的青藤碱含量

目的建立高效液相色谱法测定乌藤镇痛胶囊中青藤碱含量的方法。方法采用色谱柱：Shim-packCLC—ODS—C18柱（150mm×4．6mm,5μm）;流动相为甲醇-磷酸盐缓冲液（5mmol／L磷酸氢二钠溶液,以5mmol／L磷酸二氢钠调节pH值至8．0,再以1％三乙胺溶液调节pH至9．0）（55：45）;流速为1．0ml／min,柱温为25℃,检测波长为262nm。结果青藤碱在0．92～4．60μg之间线性关系较好,相关系数r=0．9996。加样回收率为99．21％（RSD为0．61％）。结论本方法灵敏、准确、快速,可用于乌藤镇痛胶囊中青藤碱含量测定及质量控制。     

HPLC法测定五甘桑冲剂中五味子甲素的含量

目的：建立高效液相色谱法测定五甘桑冲剂中五味子甲素含量的方法。方法应用甲醇超声提取五甘桑冲剂样品10min,提取液经浓缩后甲醇溶解;高效液相色谱法测定,色谱柱：Diamonsil－C18柱（250mm ×4．6mm,5μm）;流动相：甲醇－水（65∶35）;柱温25℃,流速0．8mL?min －1,进样体积10μL。结果五味子甲素在0．06～0．42mg? mL －1范围内线性关系良好,Y＝0．0414X ＋0．028,r＝0．9992,回收率为98．3％, RSD＝1．4％（n＝9）。结论所建方法便捷、专属性强,适用五甘桑冲剂中五味子甲素的含量测定。     

HPLC法测定小建中颗粒中芍药苷和肉桂酸的含量

目的：采用高效液相色谱法测定小建中颗粒中芍药苷和肉桂酸的含量。方法采用Ultimate XB－C18（4．6×250mm,5μm）色谱柱;乙腈－水（17∶83）为流动相;流速1．0mL? min －1;检测波长230nm,柱温：30℃。结果芍药苷和肉桂酸在20－200μg? mL －1（r＝0．9999）,0．2～20μg?mL －1（ r＝0．9997）范围内线性关系良好,平均加样回收率为101．58％、99．52％, RSD 分别为2．43％（ n ＝6）和2．23％（ n ＝6）。结论本法简便、准确,可作为该制剂的质量控制方法。     

HPLC法同时测定颈舒颗粒中天麻素和桂皮醛的含量

目的：建立HPLC法同时测定颈舒颗粒中天麻素和桂皮醛含量测定的方法。方法采用高效液相色谱法,色谱柱：Platisil ODS 柱（4．6mm ×250mm,5μm）,流动相：乙腈（A）－水（B）;梯度洗脱;流速1．0mL? min －1;柱温30℃;检测波长：天麻素为220nm,桂皮醛为290nm;进样量：10μL。结果天麻素和桂皮醛分别在在10．32～206．40μg? mL －1（r ＝0．9998,n＝6）、8．97～179．40μg? mL －1（r ＝0．9999,n＝6）范围内与其峰面积呈良好的线性关系。天麻素和桂皮醛的平均加样回收率分别为为100．79％、99．10％,RSD分别为1．32％、1．36％（ n＝6）。结论该方法操作准确、简便、重现性好,可用于颈舒颗粒中天麻素和桂皮醛的含量测定。     

RP －HPLC 法测定消银颗粒中绿原酸的含量

目的：建立反相高效液相色谱法测定消银颗粒中绿原酸含量的方法。方法色谱柱：Zorbax SB －C18柱,流动相：乙腈－0．4％磷酸（12∶88）,检测波长：327 nm,柱温：30℃。结果绿原酸进样量在0．0947～0．5680μg（r ＝0．9999）范围内线性关系良好,平均回收率为99．79％,RSD 值为1．86％（n ＝6）。结论该方法简便,快速,准确,适用于消银颗粒中绿原酸的含量测定。     

瑞舒伐他汀钙片的含量测定分析

目的：瑞舒伐他汀钙片含量测定分析。方法采用Waters色谱柱 C18（柱长250mm,内径4．6mm,填料粒径5μm）,水－乙腈－1％（V／V）三氟乙酸溶液（62∶37∶1）为流动相,流速为0．8mL· min －1,柱温40℃,UV检测波长为242nm,进样量10μL。结果高效液相测定的瑞舒伐他汀钙的线性范围为4．856μg· mL －1～48．56μg· mL －1（相关系数 r ＝0．9999）,线性关系良好,平均回收率为100．5％（9份回收的 RSD 为0．75％）。结论瑞舒伐他汀的高效液相色谱法测定含量方法准确可行,专属性强,操作简便,可作为瑞舒伐他汀钙片的含量分析方法。     

HPLC法测定追风活络胶囊中青藤碱的含量

目的:测定追风活络胶囊中青藤碱的含量。方法:采用高效液相色谱法。色谱柱为岛津Shim-pack VP-ODS（5μm,150mm×4.6mm）;流动相为:甲醇-水-乙二胺（500:500:0.05）;流速:1.0mL·min-1;检测波长264nm;柱温:室温。结果:青藤碱在0.2476～1.238μg范围内具有良好线性关系,平均回收率为99.8％,RSD<2.1％。结论:该法可用于追风活络胶囊中青藤碱的含量测定。     

反相高效液相色谱法测定辣椒风湿软膏中总辣椒碱含量

目的用反相高效液相色谱法（RP—HPLC法）测定辣椒风湿软膏中总辣椒碱的含量。方法采用ZorbaxC18柱（250mm×4．6mm，5pm）；流动相为甲醇-2．5％乙酸溶液（60：40），流速为2．0mL／min，检测波长为280nm，进样量为20μL。结果方法的线性范围为2-200μg／mL（r=1．0000），精密度RSD为0．45％（n=5），加样回收率为98．64％（RSD为0．72％）。结论RP～HPLC法具有专属、灵敏、快速、准确等优点，可用于辣椒风湿软膏中总辣椒碱含量的测定。     

RP—HPLC法测定盐酸青藤碱缓释片中主药的含量

目的：探讨建立反相高效液相色谱法（RP—HPLC）测定盐酸青藤碱缓释片中主药含量的方法。方法：色谱柱：KromasilC18流动相为乙腈-磷酸二氢钠水溶液（85：15）,检测波长265nm,流速1ml／min,柱温30℃,进样量20μl。结果：盐酸青藤碱检测的线性范围为20．24-202．4μg／ml（r=0．9992）,平均回收率为100．1％,RSD=0．9％。结论：本方法简便、准确、专属性强,可用于该制剂的质量控制。     

HPLC法测定胆仙胶囊中绿原酸的含量

目的：建立测定胆仙胶囊中绿原酸含量的方法。方法采用高效液相色谱法。色谱柱为依利特C18（4．6mm ×250mm,5μm）,流动相为乙腈－0．1％磷酸水溶液（20∶80,V／V）,流速为1．0mL? min －1,检测波长为327nm,进样量为10μL。结果绿原酸的质量浓度线性范围为14．0～140μg? mL－1（r＝0．9992,n＝6）;平均加样回收率为99．52％,RSD为0．73％（n＝9）。结论本方法快速、简便、准确、重现性良好,可用于该制剂的质量控制。     

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.     

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.     

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.     

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.