气相色谱法同时测定桑菊感冒片中α-蒎烯、β-蒎烯、(-)-薄荷酮和薄荷脑含量

目的建立GC-FID法同时测定桑菊感冒片中α-蒎烯、β-蒎烯、(-)-薄荷酮和薄荷脑的含量。方法采用HP-5石英毛细管色谱柱(30 m×0.32 mm,0.25μm)程序升温,流速1.5 mL·min~(-1),分流比30∶1,进样量1μL。结果α-蒎烯、β-蒎烯、(-)-薄荷酮和薄荷脑分别在质量浓度0.256 8～25.68 mg·L~(-1)(r=0.999 5)、1.040～104.0 mg·L~(-1)(r=0.999 5)、1.643～164.3 mg·L~(-1)(r=0.999 5)和2.302～230.2 mg·L~(-1)(r=1.000)内线性关系良好,平均回收率分别为96.1%、96.4%、96.8%和96.7%,RSD分别为1.7%、1.9%、1.2%和2.3%。结论本方法可为桑菊感冒片的质量控制提供科学依据。     

GC法同时测定薄荷桉油含片(Ⅱ)中桉油精、(-)-薄荷酮、薄荷脑的含量

目的 建立GC法同时测定薄荷桉油含片(Ⅱ)中桉油精、(-)-薄荷酮、薄荷脑的含量，以达到全面控制该药品质量。方法 采用气相色谱仪，毛细管柱为Agilent HP-INNOWAX(30 m×0.25 mm, 0.25μm),程序升温，以氮气为载体，采用氢火焰离子检测器，进样口温度220℃,检测器温度250℃,流量1.2 mL·min^-1,进样量1μL,分流比10∶1。结果 在该色谱条件下，桉油精，(-)-薄荷酮和薄荷脑分离度良好，质量浓度分别在49.2～1179.8μg·mL^-1、20.4～489.6μg·mL^-1、231.7～5560.9μg·mL^-1范围内与峰面积呈良好的线性关系，平均回收率分别为100.62%、100.36%、99.69%。结论 本方法操作简便，结果准确，重现性好，通过多组分的含量测定控制薄荷桉油含片(Ⅱ)的质量，可用于提高该药的质量标准。     

气相色谱法测定爽肤洗液中薄荷酮和薄荷脑的含量

目的 建立爽肤洗液中薄荷酮和薄荷脑含量测定的方法.方法 采用气相色谱法测定爽肤洗液中薄荷酮和薄荷脑的含量,色谱柱:Agilent DB-WAX毛细管柱(30 m×0.32 mm,0.5μm);程序升温.进样口温度:220℃;检测器:FID,温度为250℃.结果 (-)-薄荷酮和薄荷脑分别在0.04908~0.9816、0.0449~0.8980μg范围内呈较好的线性关系,r分别为0.9991、0.9995,均精密度RSD<1.0%,平均加样回收率分别为98.76%、99.60%,RSD分别为2.25%、1.96%.结论 该实验建立的方法易操作,重现性好,可以用来同时测定爽肤洗液中薄荷酮和薄荷脑的含量.     

高效毛细管气相色谱法测定保心安油中（—）—薄荷酮、薄荷脑和桂皮醛的含量

目的:采用高效毛细管气相色谱法同时测定保心安油中(-)-薄荷酮、薄荷脑和桂皮醛的含量。方法:采用HP-INNOWAX毛细管柱(Crosslinked Polyethylene Glycol,0.25μm× 0.25 mm×30m),GC-MS分离鉴定保心安油10种成分,3种成分的含量采用内标法测定,用HP-FFAP毛细管柱(Crosslinked Polyethylene,0.25μm×0.25 mm×30 m),柱温:115℃ 4℃min~(-1)155℃(1 min)40℃min~(-1)230℃(4min),分流进样,分流比40:1;进样口温度:180℃;检测器:FID,温度:250℃。结果:3种成分均达到良好的分离,(-)-薄荷酮、薄荷脑和桂皮醛线性范围分别为0.83～4.16μg(r=0.999 9),2.52～12.60μg(r=0.999 9),0.20～1.00μg(r=0.999 9);重现性均小于1.5％,平均回收率分别为(-)-薄荷酮:99.18％,RSD=1.4％;薄荷脑:99.92％,RSD=1.1％;栓皮醛:99.22％,RSD=1.4％。     

气相色谱法测定复方苦参凝胶中薄荷酮、薄荷脑的含量

目的建立复方苦参凝胶中薄荷酮、薄荷脑的含量测定方法。方法采用GC法测定薄荷酮、薄荷脑的含量,色谱柱为弹性石英毛细管柱（柱长30m,内径0．32mm,膜厚度0．25μm）Supelcowax-10;程序升温;进样口温度260℃,检测器温度280℃;分流比50：1;柱流量1．0mL·min^-1。结果采用C-C法测定薄荷酮、薄荷脑的含量,薄荷酮的量在0．0562～0．4215μg有良好的线性关系（r=0．9997）,平均回收率为97．12％,RSD=1．55％;薄荷脑的量在0．03216～0．2412μg有良好的线性关系（r=0．9992）,平均回收率为98．17％,RSD=1．70％。结论所建立的含量测定方法简便可行、重复性好,可以用来测定复方苦参凝胶中薄荷酮、薄荷脑的含量。     

UPLC同时测定不同产地川芎中8种活性成分的含量

目的建立同时测定不同产地川芎中咖啡酸、香草醛、阿魏酸、洋川芎内酯I、洋川芎内酯H、丁基苯酞、藁本内酯和丁烯基苯酞含量的UPLC方法。方法采用ACQUITY UPLC,HSS T3色谱柱(2.1 mm×100 mm,1.8μm),流动相为甲醇-0.03%磷酸水溶液,梯度洗脱,PDA检测器,针对不同组分,选择其最大吸收波长作为检测波长。结果咖啡酸、香草醛、阿魏酸、洋川芎内酯I、洋川芎内酯H、丁基苯酞、藁本内酯和丁烯基苯酞分别在0.082 8～3.312μg.mL 1,0.047 85～1.914μg.mL 1,4.420～176.8μg.mL 1,2.035～81.4μg.mL 1,0.470 4～18.82μg.mL 1,1.044～41.75μg.mL 1,13.55～542.0μg.mL 1,1.785～71.40μg.mL 1内呈良好的线性关系,平均回收率分别为101.0%,99.1%,98.9%,103.6%,96.3%,102.8%,98.1%,98.0%。结论该方法简便、快捷、重复性好,可用于川芎药材及其制剂的质量控制。     

GC法测定爽肤洗液中薄荷酮和薄荷脑的含量

目的:建立爽肤洗液中薄荷酮和薄荷脑含量测定的方法。 方法:采用气相色谱法测定爽肤洗液中薄荷酮和薄荷脑的含量,色谱柱：Agilent DB-WAX毛细管柱（30 m×0.32 mm,0.5 μm）;程序升温。进样口温度：220 ℃;检测器：FID,温度为250 ℃。 结果:(-)-薄荷酮和薄荷脑分别在0.04908~0.9816 μg、0.0449~0.898 μg范围内呈较好的线性关系,r分别为0.9991、0.9995,精密度RSD均＜1.0 %,平均加样回收率分别为98.76%、99.60%,RSD 分别为 2.25%、1.96%。 结论:本实验建立的方法易操作,重现性好,可以用来同时测定爽肤洗液中薄荷酮和薄荷脑的含量。     

GC-FID法测定消癥丸中莪术酮、藁本内酯和α-香附酮

目的 建立气相色谱–氢火焰离子化检测器（GC-FID）法同时测定消癥丸中莪术酮、藁本内酯和α-香附酮的方法。方法 采用HP-5MS毛细管柱（30 m×0.25 mm×0.25 μm）,FID检测器：280℃,进样口温度240 ℃;程序恒温130 ℃,保持45 min;载气为N₂,柱体积流量1.5 mL/min,不分流模式;进样量：1 μL。结果 莪术酮、藁本内酯、α-香附酮分别在1.684～168.400、2.496～249.600、2.180～218.000 μg/mL线性关系良好;平均回收率分别为97.98%、99.76%、96.06%,RSD值分别为1.62%、0.89%、1.29%。结论 该方法操作简单、重复性好,可为评价消癥丸的质量控制提供依据。     

HPLC法同时测定当归药材中6种成分的含量

目的:建立高效液相色谱法同时测定当归药材中阿魏酸、阿魏酸松柏酯、Z 型和 E 型藁本内酯及 Z 型和 E 型3-丁烯基苯酞的含量。方法:采用 Zorbax ODS C_(18)色谱柱(250 mm×4.6 mm,5 μm);流动相为1%醋酸(A)-乙腈(B),梯度洗脱(0min,10%B;7 min,33%B;55 min,33%B),流速1.0 mL·min~(-1);检测波长为324 nm(阿魏酸、阿魏酸松柏酯和 Z/E 型藁本内酯)和260 nm(Z 型和 E 型3-丁烯基苯酞)。结果:阿魏酸、阿魏酸松柏酯、Z-藁本内酯、Z 型和 E 型3-丁烯基苯酞的线性范围分别为3.31～139.50 μg·mL~(-1)(r=0.9999),38.00～380.00 μg·mL~(-1)(r=0.9995),2.11～445.00 μg·mL~(-1)(r=1.000),3.32～136.18 μg·mL~(-1)(r=0.9999),1.94～16.32 μg·mL~(-1)(r:0.9995);加样回收率分别为101.8%(RSD=2.5%),105.3%(RSD=3.2%),98.5%(RSD=1.6%),105.3%(RSD=2.4%),105.8%(RSD=1.9%)。结论:该方法准确、简便,具有良好的重复性和稳定性,有利于提高当归药材的质量控制。     

气相色谱法测定薄荷素油中薄荷脑、薄荷酮、薄荷脑乙酸酯、柠檬烯的含量

目的采用高效毛细管柱气相色谱法同时测定薄荷素油中主要成分薄荷脑、薄荷酮、薄荷脑乙酸酯、柠檬烯含量。方法色谱柱:HP-FFAP毛细管柱(25m×0.20mm×0.33μm),60℃～230℃程序升温,内标物环己酮。结果各组分线性关系良好,相关系数为1.0000。加样回收率:薄荷脑97.71%,薄荷酮102.18%,薄荷脑乙酸酯98.20%,柠檬烯97.30%。结论该方法简便、准确、可靠,可作为控制薄荷素油质量的方法。     

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.     

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.