HPLC法同时测定复方水杨酸搽剂中三组分的含量

目的：建立高效液相色谱法同时测定复方水杨酸搽剂中3组分含量的方法。方法：采用Hypersil BDS C18（4．6mm×200mm，5μm）色谱柱，0．1mol·L^-1磷酸氢二钠溶液-甲醇（60：40，用20％磷酸调节pH5．0）为流动相，流速为1．0mL·min^-1，检测波长为212nm。结果：间苯二酚、水杨酸、苯酚分别在0．0388—0．776μg（r=0．9999），0．1176～2．352μg（r=0．9999）、0．0218～0．436μg（r=0．9999）范围内线性关系良好，3个浓度组间苯二酚的平均回收率分别为99．0％（RSD=0．3％），97．2％（RSD=0．5％），98．5％（RSD=0．8％），水杨酸的平均回收率分别为100．3％（RSD=0．4％），99．5％（RSD=0．7％），97．5％（RSD=0．6％），苯酚的平均回收率分别为97．1％（RSD=1．1％），97．8％（RSD=0．7％），99．6％（RSD=0．9％）。结论：本测定方法简便、快速、准确，为复方水杨酸搽剂质量评价提供了可靠方法。     

高效液相色谱法测定参麦注射液3种人参皂苷的含量

目的：建立参麦注射液中3种人参皂苷Rg1、Re和Rb1的含量测定方法。方法：高效液相色谱法，色谱柱为C18柱，以乙腈为流动相A，水为流动相B，进行梯度洗脱。检测波长为203nm。结果：人参皂苷Rg1、Re和Rb1的线性范围分剐为0．4810～4．810μg，0．4025～4．025μg和0．6005～6．005μg。平均回收率分别为99．88％（RSD为0．34％，n=6），99．69％（RSD为0．36％，n=6）和99．59％（RSD为0．43％，n=6）。结论：本法简单、快速，结果准确。     

导数光谱法测定复方氯霉素鱼肝油搽剂中氯霉素的含量

目的：建立复方氯霉素鱼肝油搽剂中氯霉素的含量测定方法。方法：采用一阶导数分光光度法不经分离直接测定氯霉素的含量，检测波长为278nm。结果：氯霉素在浓度为12-28μg／ml内呈线性范围，相关系数r=0．9999。浓度为12、20、28μg／ml的样品液，日内RSD分别为1．00％、1．11％和1．13％，日间RSD分别为1．35％、1．84％和1．67％。浓度为12、16、20、24μg／ml样品液的平均回收率分别为101．58％、99．9％、98．9％、101．13％，RSD值为1．21％。结论：本方法可消除其他组分的干扰，简便易行，适合医院制剂的含量测定。     

气相色谱法测定伤痛平膏中水杨酸甲酯、薄荷脑、辣椒素的含量

目的：建立气相色谱法测定伤痛平膏中水杨酸甲酯、薄荷脑、辣椒素含量。方法：采用hp-5毛细管柱；柱温90～180℃；进样口温度250℃；FID检测器，检测器温度280℃。结果：水杨酸甲酯线性范围为0．76～7．56μg，平均加样回收率为100．5％，RSD为0．52％（n=5）；薄荷脑线性范围为0．25～2．54μg，平均加样回收率为99．4％，RSD为0．78％n=5）；辣椒素线性范围为0．503～5．03μg．平均加样回收率为100．2％，RSD为0．88％（n=5）。结论：本方法测定结果准确可靠，可用于测定伤痛平膏中水杨酸甲酯、薄荷脑、辣椒素的含量。     

高效液相色谱法定量分析黄芩苷粗品中4种黄酮类成分

目的：建立黄芩苷粗品中黄芩苷、黄芩素、汉黄芩苷和汉黄芩素含量的高效液相色谱（HPLC）测定方法，以便控制其质量。方法：固定相用Agilent ZORBAX SB-C18柱（5μm，4．6mm×250mm），苷流动相为甲醇-水-冰醋酸（49：51：0．2），苷元流动相为甲醇-水-冰醋酸（61：39：0．2），检测波长为275nm。结果：黄芩苷、黄芩素、汉黄芩苷和汉黄芩素线性范围分别是0．102～1．020μg（r=0．9997），0．051～0．510μg（r=0．9994），0．01～0．51μg（r=0．9995），0．02～0．20μg（r=0．9999）；平均回收率（n=5）分别为99．12％（RSD为1．55％），101．60％（RSD为2．67％），102．27％（RSD为1．92％／40）和98．51％（RSD为3．13％）。结论：本方法简便、准确，可用于黄芩苷粗品的质量控制。     

HPLC法测定畅心通滴丸中黄酮醇苷含量

目的：建立畅心通滴丸中黄酮醇苷的含量测定方法。方法：采用高效液相色谱法，色谱柱为迪马Diamonsil^TM C18柱（4．6mm×250mm，5μm），流动相为甲醇-0．5％磷酸水溶液（52：48），流速1．0mL·min^-1，柱温35℃，检测波长为360nm。结果：槲皮素、山柰素、异鼠李素峰的线性范围分别为0．060～0．54μg、0．059～0．53μg、0．042～0．37μg，相关系数为0．9998～0．9999，平均加样回收率（n=9）分别为100．0％（RSD=2．5％）、100．0％（RSD=2．4％）、100．0％（RSD=2．2％）。结论：本方法快速简便，结果准确，为质量标准提供了科学依据。     

分光光度法测定复方酮替芬喷鼻剂中酮替芬的含量

目的：建立复方酮替芬喷鼻剂中酮替芬的含量测定方法。方法：采用紫外分光光度法不经分离直接测定酮替芬的含量，检测波长为301nm。结果：酮替芬在浓度为5～30μg／ml内呈线性，相关系数r=0．9999。浓度为7．5、15、30μg／ml的样品液，日内RSD分别为2．68％、1．00％和1．61％，日问RSD分别为2．80％、0．90％和0．81％。浓度为7．5、15、30μg／ml的样品液的平均回收率分别为99．12％、100．25％、99．62％，RSD分别为3．56％、2．10％和1．93％。结论：本方法简便易行，适合复方酮替芬喷鼻剂中酮替芬的含量测定。     

复方甲硝唑醇溶液中甲硝唑、水杨酸的含量测定

目的：测定复方甲硝唑醇溶液中甲硝唑、水杨酸的含量。方法：采用双波长分光光度法同时测定甲硝唑、水杨酸的含量。结果：甲硝唑的线性范围为6．9～16．1μg／mL，平均回收率为99．83％，RSD为1．28％；水杨酸的线性范围为3．3—7．7μg／mL，平均回收率为96．48％，RSD为0．84％。结论：双波长分光光度法简便、快速、准确，适用于复方甲硝唑醇溶液的分析检测。     

HPLC-ELSD法测定银杏达莫注射液中萜类内酯的含量

目的建立银杏达莫注射液中白果内酯、银杏内酯A、银杏内酯B及银杏内酯C4种成分的反相高效液相色谱分析方法。方法采用大连江申Hypersil ODS2柱（200mm×4．6mm，5μm），四氢呋喃-甲醇-水（1：22：77）为流动相，流速为1．0mL·min^-1柱温：（35±0．1）℃；ELSD参数：漂移管温度为94℃，气体压力为50psi。结果白果内酯、银杏内酯A、银杏内酯B及银杏内酯C分别在4．25～16．5μg；3．74～14．52μg；3．58～13．86μg；3．40～13．20μg内呈良好的线性关系，且4种成分的平均回收率分别为100．3％（RSD=0．76％），100．0％（RSD=0．39％），99．8％（RSD=0．48％），99．9％（RSD=0．70％）。结论所建立的HPLC-ELSD法具有较好的精密度和重现性，可用于银杏达莫注射液的质量控制。     

高效液相色谱法和微生物法测定人血浆中哌拉西林浓度的比较

目的：比较HPLC法和微生物法测定血浆中哌拉西林浓度的差异。方法：6名健康志愿单剂量静脉滴注哌拉西林4g，分别用HPLC法和微生物法测定血浆中药物浓度。结果：HPLC法线性范围为0．5－500μg/ml，回收率为97．40％－100．06％，日内、日间RSD分别为2．58％－3．24％和3．32％－5．59％，微生物法线性范围为0．5－10μg/ml，回收率为98．38％－106．85％，日内，日间RSD分别为3．90％－6．37％和7．07％－9．78％。结论：两种方法回收率和精密度均符合要求，受试各时间点平均血药浓度无显性差异。     

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.