HPLC法测定健脑合剂中氨基比林和咖啡因的含量

目的：建立高效液相色谱法测定健脑合剂中氨基比林加咖啡因的含量。方法：采用Ｓｐｈｅｒｉｓｏｒｂ Ｃ１８柱,以０．０２５ｍｏｌ．Ｌ＾－１磷酸（用三乙胺调节ＰＨ至３．０）－乙腈（８６：１４）为流动相,流速为０．８ｍｌ．ｍｉｎ＾０－１,检测波长２７３ｎｍ。结果：氨基比林加咖啡因分别在９０～２１０μｇ‘ｍｌ＾－１、１８～４２μｇ．ｍｌ＾－１的范围内呈良好的线性关系,平均回收率分别为１００．３％（ＲＳＤ＝０．     

反相高效液相色谱法同时测定苯巴比妥和卡马西平血药浓度

目的：建立同时测定微量血浆中苯巴比妥和卡马西平浓度的方法。方法：采用ＲＰ－ＨＰＬＣ法,以艾司唑仑为内标,同时测定微量血浆中苯芭巴比妥和卡马西平浓度。色谱柱ｓｈｉｍａｄｚｕ ｓｈｉｒｍｐａｃｋ ＣＬＣ－Ｃ１８不锈钢柱,流动相为醇－水（６０：４０）,流速０．８ｍｌ．ｍｉｎ＾－１,检测波长２５４ｎｍ。结果：苯巴比妥在４～６０μｇ．ｍｌ＾－１浓度范围内线性良好（ｒ＝０．９９９８）,卡马西平在２～１６μｇ．ｍｌ＾－１浓度范围内线性良好（ｒ＝０．９９９５）,最低检测限分别为１１．５７ｎｇ．ｍｌ＾－１和４．９２ｎｍ．ｍｌ＾－１,两者高、中、低３种浓度的平均回收率分别为９９．９２％,１０１．３０％,９７．９２％和９９．４１％,１０１．５２％,９８．２２％（ｎ＝９）,日内ＲＳＤ分别为３．１％,２．６％,３．８％和１．９％,１．６     

重组人胰岛素类似物的HPLC分析

目的：探讨ＨＰＬＣ分析在重组人胰岛素类似物临别和杂质检测中的适用性。方法：采用反相然谱柱（Ｃ１８）,以硫酸钠－磷酸缓冲液（０．２ｍｏｌ．Ｌ＾－１,ｐＨ２．３）和乙腈为流动相,流速０．８或１．０ｍＬ．ｍｉｎ＾－１,柱温４０℃,检测波长２１４ｎｍ;用分子筛柱（Ｚｏｒｂａｘ ＧＦ２５０）以磷酸铵缓冲液（０．１ｍｏｌ．Ｌ＾－１,ｐＨ７．５）和乙腈为流动相,流速０．５ｍＬ．ｍｉｎ＾－１,检测波长２１４ｎｍ;     

高效液相色谱法测定醋氯芬酸肠溶片的含量

目的：建立高效液相色谱法测定醋氯芬酸肠溶片的含量。方法：采用Ｚｏｒｂａｘ ＳＢ－Ｃ１８色谱柱,以乙晴－四氢呋喃－冰醋酸（２５：２５：５０,用０．１ｍｌ．Ｌ＾－１的氢氧化钠溶液调（ｐＨ５．５）为流动相,流速为１．０ｍｌ．ｍｉｎ＾－１,以对羟基联苯为内标物,检测波长为２７５ｎｍ。结果：醋氯芬酸在１０．２－５０．１μｇ．ｍｌ＾－１范围内呈良好线性（＝０．９９９ ３）,平均回收率为９９．８％,ＲＳＤ为１     

HPLC法测定盐酸吡格列酮片的含量

采用反相 ＨＰＬＣ法,以Ｃ１８为固定相,乙腈－１０ｍｍｏｌ／Ｌ醋酸铵缓冲液（ｐＨ ６．０）（６０： ４０）为流动相,检测波长为２２９ｎｍ,流速为１．０ｍｌ／ｍｉｎ,测定了盐酸吡格列酮片的含量。线性范围为１０～２００μｇ／ｍｌ,平均回收率为９９．７３％（ＲＳＤ＝１．２２％）。     

高效离子对液相色谱法测定促甲状腺激素释放激素（TRH）血药浓度的研究

报告反相离子对高效液相色谱法测定兔血浆中促甲状腺激素释放激素（ＴＲＨ）的浓度。采用ＯＤＳ色谱柱，流动相为０．０２ＮＨＡＣ：乙腈：庚烷磺酸（８９．８５：１０：０．１５），流速１．５ｍｌ／ｍｉｎ，检测波长为２２０ｎｍ。平均回收率１０１．６９％，ＲＳＤ为１．２８％。本法操作简便，结果准确，重现性好。     

高效液相色谱法测定血浆中曲尼司特浓度

用高效液相色谱法测定血浆中曲尼司特浓度。色谱条件：色谱柱为ＳｐｈｅｒｉｓｏｒｂＣ＿（１８）柱；乙腈－０．０１ｍｏｌ／Ｌ磷酸二氢钾溶液（３０：７０）为流动相；流速为１．２ｍｌ／ｍｉｎ；检测波长３３３ｎｍ。线性范围１—６０μｇ／ｍｌ；最小检出量为０．５μｇ，平均回收率为９１．４％。     

高效液相色谱法测定复方盐酸万乃洛韦滴眼液的含量

目的：测定复方盐酸万乃洛韦滴眼液中盐酸万乃洛韦和氧氟沙星的含量。方法：采用高效液相色谱法,色谱柱为Ａｌｌｔｉｍａ Ｃ８柱;相为０．０２ｍｏｌ．Ｌ＾－１,磷酸二氢钾－乙腈（４：１）,流速为１ｍｌ．ｍｉｎ＾－１,检测波长为２５０ｎｍ。结果：盐酸万乃洛韦和氧氟沙星的回收率分别为９９．４％,ＲＳＤ＝０．９８％,１００．２％,ＲＳＤ＝０．５７％,结论：方法快速,准确,可作为该制剂的质控标准。     

头孢他啶及有关物质的HPLC测定

采用Ｓｈｉｍ－ＰａｃｋＯＤＳ柱，以三乙胺醋酸溶液—水—乙腈（６９２４７０）（ｐＨ４．９）为流动相，流量１．０ｍｌ／ｍｉｎ，室温操作，检测波长２５４ｎｍ，在对头孢他啶及各有关物质作ＨＰＬＣ分离的同时，分别测定头孢他啶与吡啶的含量。线性范围分别为：５０～１５０ｍｇ／ｍｌ（ｒ＝１．００００）；０．５～１２．５μｇ／ｍｌ（ｒ＝０．９９８７）。ＲＳＤ分别为０．５％、３．４％。吡啶最低检测限：３．５ｎｇ。方法简便，准确     

反相离子对色谱法测定复方中右美沙芬、布洛芬含量

目的：测定复方中右美沙芬、布洛分的含量。方法：采用反相ＨＰＬＣ,以Ｓｈｉｍ－ｐａｃｋ ＣＬＤ－ＯＤＳ柱为色谱柱,乙腈－水（６５：３５,含０．００７ｍｏｌ．Ｌ＾－１ＳＤＳ,０．００７ｍｏｌ．Ｌ＾－１硝酸铵,用冰醋酸调ｐＨ至３．４）为流动相,对乙酰氨基酚为内标,于２７０ｎｍ波长处测定。结果：右美沙芬在０．０２～０．１０ｍｇ．;ｍｌ＾－１范围内呈线性关系,平均回收率为９９．２％,ＲＳＤ＝１．１％;布洛芬     

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.