HPLC法测定胃健宁胶囊中和厚朴酚及厚朴酚的含量

目的建立胃健宁胶囊中和厚朴酚及厚朴酚的检测方法。方法色谱条件为C18色谱柱;流动相:乙腈-水-冰醋酸(60∶40∶1)(V∶V∶V);流速:1.000 mL·min-1;检测波长:294 nm。结果胃健宁胶囊中和厚朴酚在0.02⁰.32μg(r=0.999 6)范围内线性关系良好,平均回收率为96.58%,RSD为1.78%(n=9);厚朴酚在0.019 60.32μg(r=0.999 6)范围内线性关系良好,平均回收率为96.58%,RSD为1.78%(n=9);厚朴酚在0.019 6⁰.313 6μg(r=0.999 8)范围内线性关系良好,厚朴酚的平均回收率为97.29%,RSD为1.39%(n=9)。结论该方法简便,准确度高,可有效控制胃健宁胶囊的质量。     

不换金正气散质量标准研究

制定不换金正气散的质量标准。对广霍香、苍术、陈皮进行了薄层鉴别。用高效液相色谱法测定制剂中厚朴酚与和厚朴酚的含量。通过方法学验证，三个薄层鉴别专属性强；厚朴酚在0．0622～0．5598pg范围内、和厚朴酚在0．0446～0．4014μg范围内，呈良好的线性关系。厚朴酚的平均回收率为100．2％（n=9），RSD为1．5％，和厚朴酚的平均回收率为99．89／5（n=9），RSD为1．6％。方法简便、准确、重现性好。可用于控制不换金正气散质量。     

HPLC法测定藿香正气片中厚朴酚与和厚朴酚的含量

目的 建立测定藿香正气片中厚朴酚与和厚朴酚的含量。方法 采用高效液相色谱法、以ODSC18为色谱柱,甲醇-乙腈-水(48;22：30)为流动相,检测波长294nm。结果 藿香正气片中厚朴酚的含量在11．36μg～56．80μg范围内线性关系良好(r=0．9992)、和厚朴酚(在5．20g～26．00g范围内)线性关系良好(r=0．9993),厚朴酚平均回收率100．8％,RSD=1．67％,和厚朴酚平均回收率101.2％,RSD=1.38%,结论 本方法测定简便、快速,测定结果准确。     

HPLC法测定金甲排石胶囊中厚朴酚与和厚朴酚的含量

目的建立测定金甲排石胶囊中厚朴酚与和厚朴酚含量的HPLC测定方法。方法采用Shim-pack VP-ODS C18柱,甲醇-水（78：22）为流动相,检测波长为294nm,流速1．0ml／min。结果厚朴酚在0．56μg～1．68μg范围内与峰面积呈良好线性关系,r=0．9999,平均加样回收率为99．40％,RSD为1．4％（n=6）;和厚朴酚在0．116μg～0．347μg范围内与峰面积呈良好线性关系,r=0．9999,平均加样回收率为99．26％,RSD为1．6％（n=6）。结论该方法简便、准确,专属性强,重现性好,可用于金甲排石胶囊的质量控制。     

复方运脾口服液的制备及质量控制

目的：探索复方运脾口服液的制备及定量方法。方法：采用反相高效液相色谱法测定复方运脾口服液中的厚朴酚、和厚朴酚的含量,色谱柱Hypersil ODS2（250mm×4．6mm,5μm）;流动相为乙腈-水-冰醋酸-三乙胺（60：37：2：1）;柱温为室温;紫外检测波长294nm。流速1ml·min^-1。结果：厚朴酚在1．0～20．0μg·ml^-1的浓度范围内线性关系良好,r=0．9999（n=6）,平均回收率为98．6％,RSD为0．59％;和厚朴酚在0．50～10．0μg．ml^-1的浓度范围内线性关系良好,r=0．9996（n=6）,平均回收率为98．6％,RSD为0．35％。结论：该方法简便、结果准确、分离度高,可作为该制剂质量标准的内容。     

HPLC法测定舒肝健胃丸中厚朴酚与和厚朴酚的含量

建立HPLC法测定舒肝健胃丸中厚朴酚与和厚朴酚的含量.采用Eclipse XDB-C18色谱柱;流动相为乙腈-水-冰醋酸(60∶38∶2);检测波长为294nm;流速为0.8ml·min-1.厚朴酚在0.02～0.11mg·ml-1,r=0.9999的浓度范围内线性关系良好,平均回收率为97.9 %,RSD为1.52 %;和厚朴酚在0.02～0.12 mg·ml-1,r=0.9999的浓度范围内线性关系良好,平均回收率为99 .0%,RSD为1.89 %.该法快捷、简便、准确,可作为该制剂的质量控制.     

高效液相色谱法测定香砂养胃丸中厚朴酚与和厚朴酚的含量

目的:建立和改进香砂养胃丸含量测定方法。方法:以Hypersil ODS C_(18)(5μm,150 mm×4.6mm)色谱柱分离厚朴酚 与和厚朴酚,流动相乙腈-水-冰醋酸(50:8:2),检测波长294nm。结果:线性范围:厚朴酚1.12～5.60μg,r=0.9999(n=5),和厚朴酚0.8288～4.144μg,r=0.9999(n=5)。厚朴酚平均回收率99.1％,RSD=1.64％(n=5),和厚朴酚平均回收率102.4％,RSD=1.67％(n=5)。结论:本法简便,快速,准确,可作为该制剂质量控制的方法。     

厚术胶囊质量标准研究

目的:建立厚术胶囊的质量标准。方法:采用薄层色谱(TLC)法对方中苍术、三七、白芍和山楂药材进行定性鉴别;采用高效液相色谱法测定厚朴中厚朴酚、和厚朴酚的含量。结果:TLC斑点清晰,阴性对照无干扰。厚朴酚与和厚朴酚的进样量分别在0.080～0.400μg(r=0.9999)、0.048～0.240μg(r=0.9999)范围内与各自峰面积积分值呈良好的线性关系;平均回收率分别为98.42%、98.34%,RSD分别为0.63%、0.90%(n=6)。结论:所建标准可有效控制厚术胶囊的质量。     

香连理气丸的质量标准研究

目的建立香连理气丸的质量标准。方法采用显微鉴别处方中的厚朴、广藿香、甘草;采用薄层色谱法对黄连、木香和厚朴进行定性鉴别,采用高效液相色谱法测定香连理气丸中厚朴的含量。结果薄层色谱斑点清晰,专属性强;和厚朴酚在6.152~92.28μg/mL的范围内、厚朴酚在8.867~133.01μg/mL的范围内呈良好线性关系,香连理气丸中和厚朴酚平均回收率为98.95%（RSD=0.9%,n=9）,厚朴酚平均回收率为99.30%（RSD=1.2%,n=9）。结论本质量标准方法简单、操作简便、结果准确、重现性好,可用于香连理气丸的质量控制。     

高效液相色谱法测定香砂养胃软胶囊中厚朴酚与和厚朴酚含量

目的 建立测定香砂养胃软胶囊中厚朴酚与和厚朴酚含量的高效液相色谱法.方法 色谱柱为DiamonsilTM C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-水-冰醋酸(60:38:2),流速为1.0 mL/min,柱温为25℃,检测波长为294 nm,进样量为10μL.结果 厚朴酚进样量在0.104 6～2.092μg范围内与峰面积线性关系良好,平均回收率为99.15％,RSD为0.85％(n=6);和厚朴酚进样量在0.054 8～1.096 μg范围内与峰面积线性关系良好,平均回收率为100.24％,RSD为1.11％(n=6).结论 该方法操作简单、专属性强、重现性好,能有效控制该制剂的质量.     

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.

---

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.