高效液相色谱法测定盐酸氟西汀的含量

目的建立测定盐酸氟西汀含量的高效液相色谱法。方法选用Agilent Eclipse XDB-C8柱(4.6 mm×250mm,5μm);流动相:四氢呋喃-甲醇-三乙胺缓冲液(取三乙胺10ml,置1 000ml量筒中,加水980ml,用磷酸调节pH值至6.0)(301060);流速为1.0ml/min;检测波长:227nm;进样量:10μl;柱温:25℃。结果方法的线性范围为55.17~165.51μg/ml(r=0.999 9);最低检测限:0.15μg/ml;回收率在99.9%~100.0%之间,重复性RSD为0.1%(n=6)。结论方法简便灵敏,结果准确可靠,可用于盐酸氟西汀的质量控制。     

高效液相色谱法测定左旋多巴片的有关物质

目的:采用高效液相色谱法测定左旋多巴片的有关物质。方法:采用依利特Spherisorb C18柱(5μm,150×4.6mm),以0.01mol/L磷酸二氢钾缓冲液(含0.003mol/L辛烷磺酸钠,pH3.0)-甲醇(84:16)为流动相,检测波长280nm,流速1.0ml/min,柱温30℃。结果:降解产物在该色谱条件下与左旋多巴分离良好。结论:本方法用于测定左旋多巴片有关物质,方法简便,快速,结果准确。     

HPLC法测定氨酚待因片中有关物质对氨基酚的含量

目的:建立一种用高效液相色谱法测定氨酚待因片(Ⅰ)中有关物质对氨基酚的方法。方法:选用色谱柱Anethyst C8(250mm×4.6mm,5μm);流动相为磷酸盐缓冲液-甲醇(90:10);检测波长:245nm;流速:1.0ml/min。结果:对氨基酚在1.02～30.48μg/ml浓度范围内与峰面积呈良好的线性关系(r=0.9998)。平均回收率为98.97%。结论:本方法简单、快速、结果准确可靠。     

高效液相色谱法测定克拉维丁搽剂中醋酸地塞米松含量

目的测定克拉维丁搽剂中醋酸地塞米松的含量。方法用高效液相色谱法,色谱柱为C18柱(150 mm×4.6mm,5μm);流动相为甲醇-水-冰醋酸(80200.5);检测波长为240nm;进样量20μl;柱温30℃;流速1ml/min。结果醋酸地塞米松在2.00~64.00μg/ml范围内线性关系良好,Y=0.405 2 X+0.804 2(r=0.999 9),平均回收率为99.3%,RSD=0.93%(n=9)。结论该法便捷,重现性好,适用于克拉维丁搽剂中醋酸地塞米松的含量测定。     

头孢雷特含量测定和有关物质检查的HPLC法

目的 建立头孢雷特HPLC含量测定和有关物质检查方法.方法 使用Welchrom-C_(18)柱(250mm×4.6mm,5μm),流动相为0.02mol/L磷酸二氢钠缓冲液(用磷酸调节pH至2.50)-乙腈(88:12),检测波长254nm.结果 头孢雷特在0.0102～715.4μg/ml浓度范围内有良好的线件关系(n=9),y=20230x+51110,相关系数r=0.9999,定量限为6.7ng,最低检出限为2.0ng.结论 该方法为头孢雷特含量测定和有关物质检查提供了方便、灵敏、精确、可靠的方法.     

HPLC法测定头孢羟氨苄及其有关物质含量

目的建立头孢羟氨苄有关物质的HPLC分析方法。方法采用ODS柱(Polaris250mm×4.6mm,5μm),以0.05mol/L磷酸盐缓冲液(用10mol/L氢氧化钾调节pH值为5.5)-乙腈(96∶4)为流动相,流速为0.7ml/min,检测波长为230nm。结果头孢羟氨苄、有关物质α-对羟基苯甘氨酸、7-氨基去乙酰氧基头孢烷酸(7-ADCA)的线性范围分别为0.125～1.0mg/ml(r=0.9997)、0.312～20μg/ml(r=0.9999)、0.312～20μg/ml(r=0.9999)。结论本方法可用于头孢羟氨苄及其有关物质含量的测定,方法准确、灵敏、简便。     

HPLC测定氯唑沙宗片的含量和有关物质

目的 测定氯唑沙宗片的含量和有关物质.方法 采用HPLC法,用DiamonsilTM C18(250 mm×4.6 mm,5 μm)色谱柱;流动相为0.05 mol·L-1枸橼酸缓冲液(三乙胺调pH3.5)-乙腈(60:40);流速1.0 ml·min-1;检测波长280 nm;柱温30℃;进样量20μl.结果 氯唑沙宗与其相邻杂质峰能完全分离;在24.84～496.70 μg·ml-1范围内线性关系良好(r2=0.9998).结论 所建方法简便、准确、专属性好,可用于氯唑沙宗及其制剂的含量测定和有关物质的检查.     

高效液相色谱法测定美沙拉嗪控释胶囊的有关物质

目的:建立一种高效液相色谱法测定美沙拉嗪缓释胶囊的3-氨基水杨酸等有关物质。方法:采用HPLC法。色谱柱为Thermo BDS C8柱(4.6mm×250mm,5μm)。流动相为磷酸盐缓冲液(取磷酸二氢钾1.36g和辛烷磺酸钠2.2g,加水溶解至890ml,用磷酸调节pH至2.2)-甲醇-乙腈(890:80:30),柱温30℃,流速1.2ml·min-1,检测波长为220nm。结果:3-氨基水杨酸在0.1994～1.994μg/mL浓度范围内与峰面积呈良好线性关系,r=1.0000。平均回收率96.38%,RSD为1.71%;定量限为86.69ng/ml。结论:本方法简便、灵敏、准确,能用于美沙拉嗪缓释胶囊有关物质的质量控制。     

HPLC法测定门冬氨酸洛美沙星注射液的含量和有关物质方法研究

目的 :建立高效液相色谱 (HPL C)法测定门冬氨酸洛美沙星注射液的含量和有关物质。方法 :Diamonsil C1 8色谱柱 (2 5 0 mm× 4 .6 mm ,5μm) ,以乙腈 -磷酸盐缓冲液 - 0 .0 5 mol/ L四丁基溴化铵溶液 (19∶ 81∶ 4 )为流动相 ,流速为1.0 ml/ min,用外标法测定 ,检测波长为 2 88nm。结果 :在 16～ 14 4μg/ ml的浓度范围内 ,洛美沙星的浓度与色谱峰面积呈良好的线性关系 ,r=0 .9997;回收率为 99.9% ,RSD=1.2 % ;最低检测量为 2 ng/ ml。结论 :该法准确、简便、灵敏 ,可用于门冬氨酸洛美沙星注射液的含量测定和有关物质检查。     

HPLC法测定溴丙胺太林片的含量和有关物质

目的:建立HPLC法测定溴丙胺太林片含量和有关物质的方法.方法:色谱柱:Venusil XBP C8(150mm×4.6mm,5μm);流动相:乙腈-磷酸盐缓冲液(取十二烷基硫酸钠17.3g,氢氧化钠5.0g,加水1000ml溶解,用磷酸调节pH至3.5±0.05,加水稀释至2000ml)(54:46);检测波长:254nm.结果:溴丙胺太林在0.003～3.000mg·ml-1范围内线性关系良好(r=1.0000);平均回收率为100.2%,RSD=1.1%;各杂质峰的分离度均达到要求.结论:本测定方法准确、灵敏、专属性高,可作为溴丙胺太林片的含量测定和有关物质检查方法.     

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.