薄层扫描法测定安中解毒颗粒中绿原酸的含量

目的建立测定安中解毒颗粒中绿原酸含量的方法。方法采用硅胶G薄层板,以二甲苯-乙酸乙酯-70%乙醇-甲醇(3.5∶3.5∶1∶0.6)展开,紫外透射仪在365 nm处显色定位,在λs=310 nm,λR=245 nm条件下扫描测定。结果本线性范围为0.3~3μg,r=0.9978,平均回收率为99.89%,RSD=1.81%(n=4)。结论方法简单、准确、重现性好,可用于该产品的质量控制。     

薄层扫描法测定视明口服液中黄芩苷的含量

目的:建立视明口服液中黄芩苷测定方法.方法:采用单波长反射法锯齿形薄层扫描,以乙酸乙酯-丁酮-甲酸-水(5∶3∶1∶1)为展开剂,检测波长λs=365nm,参比波长λR=275nm,测定该制剂中黄芩苷的含量.结果:线性范围0.77～1.65μg,Y=1377.6x+93.5,r=0.9993,平均加样回收率为97.19%,RSD=1.59%(n=5).结论:本法准确简便,适合该制剂中黄芩苷含量测定.     

薄层扫描法测定化痰降气胶囊中盐酸麻黄碱含量

目的 测定化痰降气胶囊中盐酸麻黄碱的含量.方法薄层扫描法,展开剂:氯仿-甲醇-浓氨水(20∶5∶0.5),显色剂:0.3%茚三酮,检测波长λs=490 nm.结果 盐酸麻黄碱在0.336～1.680 μg范围内线性良好,相关系数r=0.9978,平均回收率为99.22%,RSD=1.94%.结论 本法适用于化痰降气胶囊中盐酸麻黄碱含量测定.     

薄层扫描法测定固脾通鼻片中黄芪甲苷含量

目的测定固脾通鼻片中黄芪甲苷含量.方法 0.2%羧甲基纤维素钠作粘合剂的硅胶G薄层板;以氯仿-甲醇-水(40∶13∶1)溶液为展开剂;λs=510nm,λR=690nm.结果线性范围0.266～2.128μg(r=0.996),平均加样回收率为95.6%;RSD=2.64%(n=5).结论本法简便、准确、重现性好,可用于质量控制.     

双波长薄层扫描法测定复方替米沙坦制剂中主药的含量

目的:建立测定复方替米沙坦制剂中替米沙坦和氢氯噻嗪含量的薄层扫描法。方法:选用展开剂为乙酸乙酯-氯仿-甲醇-冰醋酸(50∶40∶10∶5),双波长反射线性薄层扫描,线性参数SX=7,狭缝为1.0mm×5.0mm,检测波长为替米沙坦λR=365nm、λS=305nm;氢氯噻嗪λR=370nm、λS=275nm。结果:替米沙坦和氢氯噻嗪的线性范围分别为1.114~5.57(r=0.9996)、3.664~18.32μg(r=0.9998);平均回收率分别为97.95%(RSD=1.30%)、98.32%(RSD=1.13%)。结论:本方法简便、快捷、准确,可用于该制剂的含量测定。     

薄层扫描法测定固脾通鼻片中黄芪甲苷含量

目的　测定固脾通鼻片中黄芪甲苷含量。方法　 0 2 %羧甲基纤维素钠作粘合剂的硅胶G薄层板 ;以氯仿 -甲醇 -水(40∶ 1 3∶ 1 )溶液为展开剂 ;λs =51 0nm ,λR=690nm。结果　线性范围 0 .2 66～ 2 .1 2 8μg(r =0 .996) ,平均加样回收率为95 6 % ;RSD =2 .64 % (n =5)。结论　本法简便、准确、重现性好 ,可用于质量控制。     

芪黄口服液中黄芪甲苷的含量测定

目的:建立薄层扫描法测定芪黄口服液中黄芪甲苷含量.方法:以氯仿-甲醇-水(65:35:10)为展开剂,采用双波长反射式锯齿扫描方式进行测定,测定波长λs=530 nm,参比波长λR=700nm.结果:黄芪甲苷在0.948～4.740μg范围内线性关系良好(r=0.998 9),平均加样回收率为98.23%,RSD=1.40%.结论:本法简便、准确、重复性好,可作为芪黄口服液的定量分析方法.     

反相高效液相色谱法测定人体血浆中表阿霉素的含量

采用反相高效液相色谱法(以柔红霉素为内标)测定血浆中表阿霉素的含量,流动相为5mmol/LH3PO4-甲醇-异丙醇-乙晴(6∶9∶7∶2,pH2.9),YWGC18不锈钢色谱柱,荧光检测波长λex=450nm,λem=530nm.血浆中样品经氯仿-甲醇-异丙醇=5∶2∶3抽提液抽提处理后进样测定.血浆中表阿霉素的浓度在0.03～2.4mg/L范围内峰面积与柔红霉素的峰面积之比呈线性关系(r=0.9998),方法对表阿霉素的平均回收率为89%～90.7%.最低检测浓度为0.01mg/L.本法灵敏度高,线性范围大,符合临床用药的血药浓度监测和药代动力学研究的分析方法要求,并用于40例已服用表阿霉素的癌症病人的血浆药物含量的测定.     

反相高效液相色谱法测定人体血浆中表阿霉素的含量

采用反相高效液相色谱法(以柔红霉素为内标)测定血浆中表阿霉素的含量,流动相为5mmol/L H3PO4-甲醇-异丙醇-乙晴(6∶9∶7∶2,pH2.9),YWG C18不锈钢色谱柱,荧光检测波长:λex=450nm,λem=530nm.血浆中样品经氯仿-甲醇-异丙醇=5∶2∶3抽提液抽提处理后进样测定.血浆中表阿霉素的浓度在0.03～2.4mg/L范围内峰面积与柔红霉素的峰面积之比呈线性关系(r=0.9998),方法对表阿霉素的平均回收率为89%～90.7%.最低检测浓度为0.01mg/L.本法灵敏度高,线性范围大,符合临床用药的血药浓度监测和药代动力学研究的分析方法要求,并用于40例已服用表阿霉素的癌症病人的血浆药物含量的测定.     

祛痹舒肩丸中延胡索乙素的含量测定

采用双波长薄层扫描法对祛痹舒肩丸中的有效成分延胡索乙素的含量进行测定.展开剂:正己烷-醋酸乙酯-浓氨试液(3:2:0.1);扫描波长:测定波长λs=515nm,参比波长λR=650nm;狭缝:0.4mm×0.4mm;线性参数:SX=3.延胡索乙素线性范围0.48～3.84μg,r=0.9994,平均回收率为100.98%,RSD为1.77%(n=8).本法重复性好,定量准确,可作为该制剂的定量分析方法.     

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.     

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.