高效液相色谱法测定复方甲硝唑乳膏中甲硝唑和乳酸环丙沙星的含量

目的:建立复方甲硝唑乳膏中甲硝唑和乳酸环丙沙星含量测定的HPLC法.方法:采用Waters Symmetry C18色谱柱(250 mm×4.6 mm,5 μm),流动相为0.05 mol·L-1枸橼酸(三乙醇胺调pH至3.5)-乙腈(82:18),检测波长为287 nm,流速为1.0 ml·min-1.结果:甲硝唑浓度在20.0～100.0 μg·ml-1范围内与峰面积呈良好的线性关系(r=0.999 9),平均回收率为98.3%RSD为0.7%(n=5);乳酸环丙沙星浓度在16.0～80.0 μg·ml-1范围内与峰面积呈良好的线性关系(r=0.999 9),平均回收率为98.6%,脚%为0.9%(n=5).结论:方法简便、快捷,结果准确,适用于该制剂的质量控制.     

HPLC法同时测定康复新液中尿嘧啶、次黄嘌呤及肌苷含量

目的:建立HPLC法同时测定康复新液中的尿嘧啶、次黄嘌呤及肌苷含量.方法:色谱柱:Wates SunfireTM C18柱(250 mm×4.6 mm,5 μm );甲醇-3%甲醇溶液(含0.07%醋酸)梯度洗脱;检测波长254 nm;进样量:10 μl.结果:尿嘧啶在4.92～34.44 μg·ml-1 (r=0.999 9),次黄嘌呤在12.43～87.06 μg·ml-1(r=0.999 9),肌苷在24.77～173.40μg·ml-1(r=0.999 9)的浓度范围内呈良好的线性关系.尿嘧啶的平均回收率为102.63%(RSD=1.78%);次黄嘌呤的平均回收率为99.13%(RSD=1.89%);肌苷的平均回收率为98.98%(RSD=1.33%).结论:该法操作简便、准确,重复性、稳定性好,可用于同时检测康复新液中尿嘧啶、次黄嘌呤及肌苷的含量.     

HPLC法测定复方呋喃西林栓的含量

目的: 建立测定复方呋喃西林栓中呋喃西林和替硝唑含量的高效液相色谱法.方法: 用C18柱为固定相,以甲醇-水(30∶70)为流动相,检测波长为263 nm.结果: 呋喃西林和替硝唑分别在9.7～22.6 μg·ml-1和192.1～448.1 μg·ml-1浓度范围内线性关系良好(r呋=0.999 8 r替=0.999 9),平均回收率分别为100.6%和100.4%,RSD为1.2%(n=5)和1.2%(n=5).结论: 用该法同时测定复方呋喃西林栓中两主药的含量简便、快速,准确可靠.     

HPLC法同时测定复方柳安咖注射液中3组分的含量

目的:建立HPLC法同时测定复方柳安咖注射液中水杨酸钠、安替比林、咖啡因3组分的含量.方法:色谱柱为Diamonsil(TM)C18(250 mm×4.6 mm,5 μm),流动相为0.05 mol·L-1磷酸二氢钾溶液(含0.12%三乙胺,用氢氧化钠试液调节pH7.0±0.05)-甲醇(69:31).检测波长为273 nm;流速1.0 ml·min-1;柱温:30℃.结果:水杨酸钠在14.18～127.60 μg·ml-1范围内线性关系好(r=0.999 8),平均回收率为99.17%,RSD=0.56%(n=6);安替比林在4.00～36.04 μg·ml-1范围内线性关系好(r=0.999 9),平均回收率为101.71%,RSD=0.41%(n=6);咖啡因在2.16～19.48 μg·ml-1范围内线性关系好(r=0.999 8),平均回收率为101.40%,RSD=0.93%(n=6).结论:本方法简便,快速,准确,重现性好,可用于复方柳安咖注射液的质量控制.     

双波长分光光度法测定复方苯甲酸酊的含量

目的:建立一种同时测定制剂中各组分含量的分光光度法.方法:采用双波长分光光度法,以75%乙醇为溶媒,不经分离直接测定复方苯甲酸酊中苯甲酸和水杨酸的含量.苯甲酸的测定波长为275 nm,参比波长为326.2 nm;水杨酸的测定波长为302 nm.结果:苯甲酸在24～96μg·ml-1浓度范围内线性关系良好(r=0.999 9),平均回收率为100.5%,RSD为0.5%,水杨酸在6～36μg·ml-1浓度范围内线性关系良好(r=0.999 9),平均回收率为99.8%,RSD为0.5%.结论:本法快速,简便,结果准确.     

RP-HPLC法同时测定人血清中阿莫西林、克拉维酸钾浓度

目的建立RP-HPLC法同时测定人血清中阿莫西林、克拉维酸钾的浓度.方法采用Luna C18色谱柱(250 mm×4.6 mm,5 μm),以 0.05 M磷酸盐缓冲液-乙腈(90∶10;磷酸调pH至2.30)为流动相,流速1 ml*min-1.检测波长为220 nm.结果CLV在 0.066～16.86 μg*ml-1,范围内有良好线性关系,r=0.999 9 (n=9);AMO在 0.12～29.45 μg*ml-1,范围内有良好线性关系r=0.999 8(n=9).本法测定血清中CLV最低检测浓度为 0.060 μg*ml-1,AMO为 0.10 μg*ml-1.(S/N≥3).平均方法回收率为 97.5%.结论本法简便,准确,重现性好,用于阿莫西林克拉维酸钾分散片人血清中血药浓度测定取得良好结果.     

HPLC法测定琥乙红霉素静脉乳剂的含量

目的:建立琥乙红霉素静脉乳剂的含量测定方法.方法:采用Agilent Zorbax SB-C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.02 mol·L-1醋酸铵缓冲盐溶液(65∶ 35),检测波长215 nm,流速为1.0ml·min-1,柱温25℃,进样量20μl.结果:琥乙红霉素在60 ～ 600 μg·ml-1的浓度范围内与峰面积呈良好的线性关系(r =0.999 1),平均回收率为97.92％,RSD为0.43％(n=9).结论:该方法简便、快速、准确,可用于琥乙红霉素的含量测定及稳定性分析.     

高效液相色谱法测定阿替洛尔注射液的含量

目的:建立离子对色谱法测定阿替洛尔注射液的含量.方法:Betasil C18(250 mm×4.6 mm,10 μm)色谱柱,磷酸氢二钾溶液-甲醇-辛烷磺酸钠(800:200:0.5)为流动相,检测波长:275 nm,流速:1.0 ml·min-1.结果:阿替洛尔在30～105 μg·ml-1浓度范围内.线性关系良好,r=0.999 8.平均回收率为99.8%(RSD=0.6%,n=9).结论:HPLC法简便快速,稳定可靠可作为阿替洛尔注射液的质量控制方法.     

HPLC法同时测定复方槐花口服液中柚皮苷和黄芩苷的含量

目的:建立HPLC法同时测定复方槐花口服液中柚皮苷、黄芩苷的含量.方法:色谱柱:Agilent ZORBAX SB- C18(250 mm×4.6 mm,5 μm);流动相:乙腈-0.1%磷酸溶液(23:77);检测波长:280 nm;流速:1.0 ml·min-1;柱温:30℃.结果:柚皮苷和黄芩苷分别在0.194～1.742 μg·ml-1(r=0.999 5,n=5)和0.419～3.773 μg·ml-1(r=0.999 8,n=5)范围内与峰面积呈良好线性关系,平均加样回收率为100.06%,RSD为1.10%(n=6)和99.27%,RSD为1.43%(n=6).结论:HPLC法操作简便,结果准确,可用于复方槐花口服液的质量控制.     

HPLC法测定复方鱼腥草合剂中绿原酸、黄芩苷的含量

目的:建立同时测定复方鱼腥草合剂中绿原酸、黄芩苷的高效液相色谱法.方法:采用Sinochrom ODS-BP(250 mm×4.6 mm,5 μm)色谱柱;流动相为甲醇:0.2%磷酸溶液,进行梯度洗脱;柱温:30℃流速为0.9 ml·min-1,检测波长为315 nm.结果:绿原酸在0.1～1.0 μg·ml-1范围内线性关系良好(r=0.999 5),平均回收率为100.26%,RSD=0.53%(n=9);黄芩苷在1.8～18.0 μg·ml-1范围内线性关系良好(r=0.996 6),平均回收率为100.04%,RSD=0.87%(n=9).结论:本方法简便易行,能够准确、快速测定复方鱼腥草合剂中的绿原酸和黄芩苷的含量.     

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.

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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.