气相色谱法测定无极膏中5种成分的含量

目的建立一种用气相色谱法测定无极膏中5种成分含量的方法.方法采用HP-INNOWAX Polyethylene Glycol(30.0 m×250 μm×0.25 μm)毛细管色谱柱,柱温采用程序升温,进样口温度200℃,FID检测器,检测器温度250℃.结果样品中5种成分完全分离且线性关系良好,樟脑、薄荷脑、龙脑、水杨酸甲酯、麝香草酚的加样回收率分别为97.3%、98.9%、98.3%、101.3%和100.8%(n=9).结论该法简便快速,结果准确,可以有效地控制质量.     

气相色谱法测定复方硝酸咪康唑软膏中5种挥发性成分的含量测定

目的建立一种用气相色谱法测定复方硝酸咪康唑软膏中5种成分含量的方法。方法采用HP2INNOWAX Polyethylene Glycol（30.0m×250μm×0.25μm）毛细管色谱柱,柱温采用程序升温,进样口温度250℃,FID检测器,检测器温度260℃。结果样品中5种成分完全分离且线性关系良好,樟脑、薄荷脑、龙脑、水杨酸甲酯、麝香草酚的加样回收率分别为97.3%、98.9%、98.3%、101.3%和100.8%（n=9）。结论该法简便快速,结果准确,可以有效地控制质量。     

GC法同时测定明目上清片中4个成分的含量

目的:建立同时分析测定明目上清片中4个活性成分(柠檬烯、薄荷酮、薄荷脑和胡薄荷酮)的方法。方法:采用GC法,色谱柱为DB-1701毛细管色谱柱(30 m×0.3 mm,0.25μm),柱温采用程序升温(80℃保持1 min,5℃.min-1上升至120℃,保持1 min,再以50℃.min-1的速率升温至220℃,保持2 min);进样口温度:180℃;检测器:FID;检测器温度:250℃。结果:柠檬烯、薄荷酮、薄荷脑和胡薄荷酮线性范围分别为0.0103～0.507 mg·mL-1(r=0.9997)、0.0105～0.501 mg·mL-1(r=0.9999)、0.0082～0.412 mg·mL-1(r=0.9991)、0.0085～0.404 mg·mL-1(r=0.9998);平均加样回收率(n=6)分别为99.1%、97.6%、98.7%、98.3%,RSD分别为1.2%、1.8%、1.4%、1.5%。结论:该方法可用于明目上清片的质量检测。     

气相色谱法测定亚微乳凝胶剂中樟脑、薄荷脑、水杨酸甲酯的含量

目的:建立气相色谱法测定亚微乳凝胶剂中樟脑、薄荷脑、水杨酸甲酯含量的方法。方法:气相色谱柱为 SE-54柱(30m×0.32 mm,0.25μm);环己酮为内标。采用 FID 检测器,进样口温度230℃,检测器温度250℃,采用程序升温,起始温度90℃,保持5 min,以10℃·min~(-1)升到150℃,保持2 min。结果:樟脑、薄荷脑、水杨酸甲酯线性范围分别为0.18～1.60 mg·mL~(-1)(r=0.9999),0.17～1.55 mg·mL~(-1)(r=0.9998),0.40～3.59 mg·mL~(-1)(r=0.9999);平均回收率分别为99.5%,99.2%,99.1%;RSD 均小于2%(n=9)。结论:本法方便,准确,重现性好,可作为本制剂的质量控制方法。     

顶空气相色谱法测定洛伐他汀原料药中的有机溶剂残留量

目的:建立测定洛伐他汀原料药中乙醇、丙酮、乙酸乙酯、甲苯4种有机溶剂残留量的方法。方法:采用顶空气相色谱法。色谱柱为DB-624石英毛细管柱,柱温采用程序升温,检测器为氢火焰离子化检测器,检测器温度为280℃,进样口温度为160℃。结果:乙醇、丙酮、乙酸乙酯、甲苯的检测浓度的线性范围分别为10.0～250(r=1.0000)、10.0～250(r=0.9999)、10.0～250(r=0.9999)、1.78～89μg.mL-(1r=0.9997);平均回收率为97.6～99.1(RSD=0.9～1.9),定量限为0.22～5.61μg.mL-1;4批样品中4种有机溶剂残留量均符合《中国药典》2005年版要求。结论:该方法操作简便、精密度好,结果准确、可靠。     

气相色谱法测定麝香草酚中的有机溶剂残留量

目的建立了麝香草酚中有机残留溶剂异丙醇的气相色谱测定法。方法采用DB-1毛细管色谱柱(30 m×0.25 mm×1μm),以氮气为载气,FID检测器,进样口温度为250℃,检测器温度为300℃。采用程序升温,柱温:40℃,保持8 m in,然后以30℃/m in的速率升至200℃,测定残留溶剂异丙醇的含量。结果线性范围为9.8~196.6μg/m l(r=0.999 7);方法的检出限(S/N=3)为1.5×10-3μg,平均回收率为98.1%,RSD为1.9%。结论本方法简便,结果准确,重现性好,可用于麝香草酚中残留溶剂异丙醇的测定。     

气相色谱法测定红花软胶囊中亚油酸的含量

目的:建立红花软胶囊中亚油酸含量的检测方法。方法:色谱柱为固定液88%二氰丙基聚硅氧烷(60 m×0.25 mm,0.20μm),检测器为氢焰离子化检测器,检测器温度280℃,进样口温度250℃,柱温控制采用程序升温,以140℃为起始柱温,保持5 min,以4℃/min升温至240℃,保持15 min。载气为氮气,载气流速:1.0 m L/min,分流比为30∶1。结果:用亚油酸甲酯作对照,其线性范围0.270 5~5.403 3 mg/m L,γ=0.999 8,平均回收率为97.02%(RSD=1.3%,n=9)。结论:该方法准确、灵敏高、重现性好,可用于红花软胶囊中亚油酸含量的测定。     

毛细管气相色谱法检测葛根素衍生物中的残留溶剂

目的:建立葛根素衍生物中二氯甲烷、丙酮、乙酸乙酯、吡啶4种有机溶剂残留量的检测方法。方法:采用气相色谱法,色谱柱为 HP-5(交联5%苯甲基聚硅氧烷)毛细管柱(30m×0.53mm×0.23μm),载气为氮气。检测器温度:250℃;进样口温度:280℃;程序升温:初始温度为36℃,保持0.5min,以每分钟3℃升至70℃,保持1min(延迟时间3min,保持250℃)。分流进样,分流比为1:100,柱前压为37.5kPa。结果:被测物均得到很好的分离,峰面积与浓度呈现良好的线性关系,精密度良好。结论:本方法简单、快捷,且灵敏度高,可用于葛根素衍生物中的残留溶剂检测。     

分散固相萃取-气相色谱法测定薰衣草中4个特征成分含量

目的:建立基于气相色谱同时测定薰衣草中樟脑、芳樟醇、乙酸芳樟酯和乙酸薰衣草酯4个特征成分含量的分析方法。方法:样品经丙酮提取,PSA+C₁₈+GCB混合型分散固相萃取剂净化后,气相色谱-氢火焰离子化检测器进行检测。色谱条件为：使用(5%-苯基)-甲基聚硅氧烷毛细管(DB-5MS,30 m×0.25 mm, 0.25μm)色谱柱,高纯氮气为载气,进样量1μL,分流比5∶1,载气流速1.5 mL·min^-1,进样口温度250℃,柱温箱程序性升温(初始温度50℃,保持2 min,然后以5℃·min^-1的速率升温至140℃,再以20℃·min^-1的速率升温至300℃),检测器温度250℃。结果:4个成分达到完全分离,无干扰峰出现,专属性好;标准工作曲线线性相关系数均大于0.999 7;优化的试验条件下,低、中、高3个添加水平下回收率在89.9%～99.1%;日内和日间RSD在1.0%～2.6%和1.8%～3.7%;方法检测限和定量限在0.818～1.49 mg·kg^-1和2.73～4....     

HPLC-ELSD法测定玉屏风口服液中黄芪甲苷的含量

目的建立玉屏风口服液中黄芪甲苷的含量测定方法。方法采用HPLCELSD法,KromasilC18(250mm×4.6mm,5μm)色谱柱;流动相为甲醇水(74∶26);流量为0.8ml·min-1;柱温为30℃;ELSD检测器检测;ELSD漂移管温度为90℃;气体流量1.48L·min-1。结果平均加样回收率为99.1%,RSD为2.76%。结论方法准确、可靠,可用于玉屏风口服液的质量控制。     

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.

---

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.