高效液相色谱法测定羧甲司坦颗粒剂中羧甲司坦的含量

目的 测定羧甲司坦颗粒剂中羧甲司坦的含量。方法 采用高效液相色谱法。色谱柱:Hypersi　C18（4.6×300mm,5μm）;流动相:pH2.0磷酸盐缓冲液;流速:1.0mL·min-1;检测波长:210nm;进样量:10μL;柱温:室温。结果 羧甲司坦进样量在2～20μg·ml-1范围内,线性关系良好（r=1.0000）,平均回收率为99.85％,RSD=0.4％（n=9）。结论 该法简便、快速,结果准确、可靠,重现性好。     

反相离子对色谱法测定羧甲司坦片和口服溶液中羧甲司坦的含量

目的：建立反相离子对色谱法,测定羧甲司坦片和口服溶液中羧甲司坦的含量。方法：采用C18柱,以含0.05％庚烷磺酸钠的0.05mol/L磷酸二氢钾溶液(用磷酸调pH2.5)为流动相．检测波长215nm。结果;该方法羧甲司坦片剂和口服溶液的回收率分别为100.3％．RSD=0.54%(n=5)．100.5%．RSD=0.70％(n=5)。结论;该法准确．可靠．专一性强,能满足制剂质量标准的要求。     

羧甲司坦口服液含量测定方法的探讨

目的:对羧甲司坦口服液中的羧甲司坦的含量测定方法进行探讨。方法:用比色法对羧甲司坦成分进行测定。结果:回收率为100.1% ,RSD为0.87% ;线性范围为120～300μg/ml。结论:该方法简单,重现性好,适合该制剂的含量测定。     

羧甲司坦缓释片的含量测定及体外释放度研究

目的 测定自制羧甲司坦缓释片的释放度,并与市售羧甲司坦片释放度比较,为处方优选提供实验依据。方法 采用紫外-可见分光光度法(UV)测定羧甲司坦缓释片释放度,检测波长为567 nm。采用桨法,以pH=6.6的磷酸盐缓冲溶液作为释放介质,转速为100 r/min进行药物释放度测定,取样时间点为1 h、2 h、4 h、6 h、8 h、12 h。结果 羧甲司坦缓释片在1.6～14.4μg/mL范围内线性良好,回归方程为：A=0.0695c-0.0898,r=0.9993,平均回收率为99.05%,RSD为1.8%,重现性良好(RSD=0.35%)。羧甲司坦缓释片2 h时累积释放接近30%,8 h时接近90%,0～12 h释药曲线符合一级释药模型。羧甲司坦普通片在1 h时累积释放超过95%。与市售普通片相比,自制羧甲司坦缓释片缓释效果明显。结论 本课题所建立的释放度及含量测定方法操作简单,方便,稳定,可靠,重现性好,可用于羧甲司坦缓释片释放度测定。自制羧甲司坦缓释片释放速度明显低于市售羧甲司坦片,缓释效果明显。     

高效液相色谱法测定羧甲司坦片的含量

目的:建立HPLC法测定羧甲司坦片的含量。方法:色谱柱为岛津VP-ODS C18柱(150 mm×4．6 mm,5μm);流动相为磷酸盐缓冲液pH 3．0;流速0．8 ml·min-1;检测波长210 nm。结果:羧甲司坦在5-25μg·ml-1浓度范围内,线性关系良好(r=0．999 5),平均回收率为99．5％,RSD为0．6％(n=5)。结论:本法简便、快速,结果准确,重现性好,可用于羧甲司坦片的含量测定。     

高效液相色谱法测定人血浆中羧甲司坦浓度

目的:建立高效液相色谱法测定人血浆中羧甲司坦浓度.方法:采用邻苯二甲醛为柱前衍生化试剂,反相高效液相色谱法检测羧甲司坦衍生物:Hypersil BDS C18柱(4.6 mm×150 mm,5 μm);流动相:甲醇-0.05 mol·L-1醋酸钠缓冲液(pH 5.9)-四氢呋喃(15:84:1);流速:1. 0 mL·min-1;进样量:5μL,使用荧光检测器检测激发波长:338 nm,发射波长:450 nm.结果:标准曲线线性、范围1.0～40.0 mg·L-1(r=0.999 9,n=6),血浆中羧甲司坦最低检测限为0.5 mg·L-1,日内RSD为0.3%～1.3%,日间RSD为0.4%～4.5%,准确度为97.9%～102.7%,羧甲司坦回收率为99.5%～103.0%.结论:该方法分离效果好,方法学结果满意,适用于人血浆中羧甲司坦的检测.     

HPLC-ELSD法测定羧甲司坦颗粒中羧甲司坦的含量

目的:利用高效液相色谱法-蒸发光散射检测器测定羧甲司坦[1]颗粒中羧甲司坦的含量。方法:用C18柱;流动相为甲醇:水(60∶40);流速为1.0ml·min-1;ELSD-2000蒸发光散射检测器漂移管温度为95℃;载气流速为2.20L·min-1。结果:进样量在2.502μg～7.506μg范围内,线性关系良好(r=0.9993),平均回收率为99.51%(RSD=0.99%)。结论:本法简便快速,结果准确、可靠、重现性好。     

羧甲司坦口服液含量测定方法的探讨

目的：对羧甲司坦口服液中的羧甲司坦的含量测定方法进行探讨。方法：用比色法对羧甲司坦成分进行测定。结果：回收率为１００．１％,ＲＳＤ为０．８７％;线性范围为１２０－３００μｇ／ｍｌ。结论：该方法简单,重现性好,适合该制剂的含量测定。     

反相离子对色谱法测定羧甲司坦的含量及有关物质

目的：采用反相离子对液相色谱法测定羧甲司坦的含量及有关物质。方法：色谱柱为Hypersil BDS柱（250mm×4．6mm，5um）以（0.125g庚烷磺酸钠，0.25g磷酸氢二钾加水250mL溶解）-0．2％二氟乙酸-乙腈（30：68：2）为流动相，流速1．0mL·min^-1，检测波长为215nm，柱温35℃。结果：羧甲司坦在25ug～200ug·mL^-1浓度范围内，线性关系良好，r=0．9999，最低检测限为1．0ng；半胱氨酸在0.4～2.5ug·mL^-1浓度范围内，线性关系良好，r=0.9999，最低检测限为1．2ng。结论：本方法简便、快速，结果准确、可靠，重现性好，可用于羧甲司坦的有关物质检查和含量测定。     

荧光分光光度法测定福多司坦片剂的含量

目的建立一种灵敏、准确的荧光分光光度法用于测定福多司坦片的含量.方法以邻苯二甲醛为衍生剂,对福多司坦进行衍生化,在λex=342 nm、λem=454nm处测定荧光强度.结果福多司坦的线性范围为0.5～6μg·ml-1,r=0.9999.平均回收率为100.3%,RSD为0.5%(n=9).结论方法简便易行,灵敏度高,重复性好,可用于福多司坦片的含量测定.     

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.