高效液相色谱法测定雷贝拉唑钠肠溶胶囊的含量和有关物质

目的:采用高效液相色谱法建立雷贝拉唑钠肠溶胶囊有关物质检查及其含量测定方法。方法:Kromasil(4.6mm×250mm,5μm)色谱柱;柱温为20℃:流动相为0.05mol.L-1磷酸二氢钾缓冲溶液(0.1mol.L-1氢氧化钠溶液调pH7.0)-乙腈(70∶30);流速为1mL.min-1;测定波长为290nm。结果:雷贝拉唑钠在50～400mg.L-1范围内线性关系良好,r=0.9998(n=5);平均回收率为99.25%,RSD为2.08%(n=9)。结论:本方法简便,迅速,准确,可靠,专属性强。     

高效液相色谱法测定人血浆中格列本脲浓度

目的:建立测定人血浆中格列本脲浓度的高效液相色谱法.方法:格列本脲血浆样品在酸性条件下以二氯甲烷-正己烷(50:50)提取,以格列齐特为内标.Nova-pakC18柱(4.6 mm×250 mm,4μm),流动相为乙腈-0.03 mol·L-1磷酸二氢钾(pH 3.0)(44:56),流速1.2 mL·min-1,检测波长228 nm.结果:标准曲线线性范围25～600μg·L-1(r=0.9992),血浆中格列本脲最低检测限为15μg·L-1.平均提取回收率为(81.9±3.6)%,平均方法回收率为(101.1±6.8)%,日内RSD≤5.0%,日间RSD≤9.1%.结论:该方法具有良好的准确性、精密性和较高的灵敏度,适用于格列本脲的药动学研究及治疗药物浓度监测.     

高效液相色谱法测定人血浆中芬太尼浓度

目的:建立高效液相色谱测定人血浆中芬太尼浓度的方法.方法:采用外标法,以Kromasil-C18(4.6 mm×250 mm,5μm)为固定相,舍0.02 mol·L-1磷酸二氢钠水溶液-乙腈(65:35)为流动相,流速1 mL·min-1,检测波长为220 nm.结果:血浆芬太尼浓度在6～300μg·L-1范围内与峰面积呈良好线性关系(r=0.999 6),最低检测浓度为5 μg·L-1,方法回收率为(92.6±1.5)%,提取回收率为(84.9±1.4)%,日内RSD为1.8%,日间RSD为2.6%.结论:本方法具有较高的准确度,线性范围宽,方法灵敏,专一性好,操作简便,适用于临床芬太尼血药浓度的测定及临床药动学研究的要求.     

反相高效液相色谱法测定血浆中吗氯贝胺浓度

目的:建立人血浆中吗氯贝胺的反相高效液相色谱检测方法.方法:血浆样品在碱性条件下(pH 11.0)用二氯甲烷提取处理.色谱柱为μ-BondapakTM C18 (3.9 mm×15 0mm,10 μm),柱温37.0 ℃,流动相为乙腈-0.067 mol·L-1磷酸二氢钾溶液(1∶5,pH 2.6),流速1.0 mL·min-1,内标为甲氧氯普胺,检测波长为240 nm.结果:吗氯贝胺在40～4 000 μg·L-1范围内线性关系良好(r=0.999 9,n=8),血浆中最小检测浓度为10 μg·L-1(S/N=3),提取回收率为96.48%～100.38%,方法回收率在99.39%～103.07%之间,日内RSD≤8.14%,日间RSD≤6.25%.结论:该方法快速、准确、灵敏度高、专一性强,可用于吗氯贝胺血浆浓度监测和药动学及生物利用度研究.     

高效液相色谱法测定血浆中尼扎替丁浓度

目的:建立测定人血浆中尼扎替丁的高效液相色谱方法.方法:采用Diamonsil C18色谱柱(200 mm×4.6mm,5μm),流动相为0.1 mol·L-1醋酸铵缓冲液-甲醇(60:40),检测波长为320nm.血浆样品加盐析溶液碱化后以氯仿提取,雷尼替丁为内标.结果:尼扎替丁血药浓度线性范围为20～6 000l·L-1(r=0.999 9,n=6),最低检测浓度为10μg·L-1(S/N=3),方法回收率在96.84%～101.39%(n=5),日内和日间RSD均小于4%.结论:本法简便,快速,重现性好,适于尼扎替丁的药动学研究.     

HPLC荧光和质谱两种检测器测定大鼠血浆及组织中的表阿霉素

目的 建立测定大鼠血浆及组织中表阿霉素浓度的方法.方法 采用RP-HPLC荧光和质谱两种检测器,Lima C18(2)分析柱(150 mm×4.6 mm,5μm),流动相为0.01 mol·L-1乙酸铵-乙腈(60:40,甲酸调pH3.5),流速0.6 ml·min-1,样品在碱性条件下,用乙酸乙酯漩涡混合提取浓集后进样,λEx=450 am,λEm=530 nm,质谱以MRM模式测定,内标法定量.结果 荧光检测标准曲线在2.44～2.50×103μg·L-1有良好线性,定量限2.44μg·L-1,日内RSD小于5.0%,日间RSD小于8.6%,方法回收率99%～113%,萃取回收率86.8%～89.7%;质谱检测标准曲线在0.49～2.00×103μg·L-1有良好线性,定量限0.49μg·L-1,日内RSD小于6.5%,日间RSD小于8.7%,方法回收率98～5%.结论 所建方法快速简便、灵敏准确,适用于血浆及组织中表阿霉素的测定及药物动力学研究.     

RP-HPLC同时测定血浆中8种苯二氮(艹卓)类药物

目的 采用HPLC法建立同时测定血浆中8种苯二氮(艹卓)类药物(氯硝西泮、艾司唑仑、阿普唑仑、三唑仑、澳沙西泮、替马西泮、氯氮(艹卓)和地西泮)的方法.方法 血浆样品经正己烷-二氯甲烷(5:3)提取.选用Diamonsil Rp-C18柱(250 mm×4.6mm,5μm);甲醇-25 mmol.L-1醋酸铵溶液(63:37)作流动相,流速1.0 mL·min-1,检测波长230 nm.结果 氯硝西泮、三唑仑、澳沙西泮、氯氮(艹卓)、地西泮的最低检测浓度为8μg·L-1,艾司唑仑、阿普唑仑、替马西泮的最低检测浓度为5μg·L-1;方法回收率接近100%;提取回收率大于70%,日内、日间精密度小于6%;艾司唑仑、阿普唑仑和替马西泮10～1.5×103μg·L-1的线性关系良好,其余5种药物的线性范围为20～1.5×103μg·L-1(r＞0.999).结论 所建方法操作简便、快速、准确、灵敏度高、重复性好,适用于临床上人血浆中8种苯二氮(艹卓)类药物的同时定性、定量检测.     

高效液相色谱-紫外检测法测定血浆多潘立酮

目的 建立HPLC-UV法测定血浆中多潘立酮浓度的方法.方法 血浆样品碱化后以有机溶剂提取;以ZORBAX SB-C18(4.6 mm×250 mm,5μm)为色谱柱;以乙腈-0.15 mol·L-1KH2PO4=30:70为流动相,检测波长为230 nm.结果 血浆浓度在1.0～128.0μg·L-1范围内线性关系良好(r=0.9996);最低检测浓度为1.0μg·L-1;高中低3个浓度的平均回收率为89.76%;日内、日间RSD均小于10%.结论 本方法灵敏度符合检测要求、干扰少、重现性好.     

高效液相色谱法测定血浆中伏立康唑的浓度

目的建立测定人血浆中伏立康唑浓度的高效液相色谱法。方法色谱柱为Hedera ODS-2(4.6 mm×250mm,5μm),流动相为:0.1 mol·L-1磷酸二氢钠-水-乙腈(20∶35∶45),流速为1.0 mL·min-1,血浆样品经乙酸乙酯-二氯甲烷(75∶25)提取后,在255 nm波长下进行检测。结果伏立康唑在0.101~12.16μg·mL-1与峰面积呈现良好的线性关系(Y=0.5345X+0.00254,r2=0.9995),相对回收率均在95%~110%,日内和日间RSD均<6%。结论该方法专属性强、灵敏度高,适合伏立康唑的血浆浓度测定及药动学研究。     

HPLC法测定围手术期患儿血浆中瑞芬太尼浓度

目的:建立高效液相色谱法测定围手术期患儿血浆瑞芬太尼浓度.方法:采用Hypersil CN柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.02 mol·L-1磷酸二氢钾水溶液内含三乙胺0.02%(30:70);流速1.0 ml·min-1;检测波长210nm;进样量为20 μl.结果:标准曲线在1.0～100.0 μg·L-1 内线性关系良好(r=0.999 3).最低检测浓度为1.0μg·L-1.提取回收率(76.51±0.82)%.方法回收率99.66%～102.40%.日内和日间RSD均小于15%.2μg·L-1组靶控浓度与实测浓度基本一致.结论:本方法快速、准确、灵敏、专一性好,适用于临床瑞芬太尼血药浓度检测和药动学研究.     

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.