高效液相色谱法测定星翳明片中丹皮酚含量

目的用高效液相色谱法测定星翳明片中丹皮酚含量。方法采用KromasilC18( 2 0 0mm×4 6mm ,5 μm)色谱柱 ,甲醇 水 (V∶V =5 8∶4 2 )为流动相 ,检测波长 2 74nm ,流速 1 0mL/min。结果线性范围 0 4 896～ 2 4 48μg(r=0 9999,n =5 ) ,平均回收率 99 1 % ,RSD为 1 2 % (n =6)。结论本法适合测定星翳明片中丹皮酚的含量。     

HPLC法测定耳聋左慈丸中的丹皮酚的含量

目的 :应用高效液相色谱法对耳聋左慈丸中的丹皮酚进行含量测定。方法 :选用RPC18分析柱 (2 5 0mm×4 6mm ,5 μm) ,甲醇 -水 -乙酸 (6 5∶30∶5 )为流动相 ,检测波长为 2 74nm ,流速为 0 8mL·min-1。结果 :线性范围为 0 0 5 2～ 0 6 2 4μg (r=0 9999) ,平均回收率为 98 72 % ,RSD为 1 8%。 结论 :本法简便、灵敏、准确。     

反相高效液相色谱法测定原料药及注射剂中丹皮酚的含量

目的　建立反相高效液相色谱法 (RP HPLC)测定原料药及注射剂中丹皮酚 (paeonol,Pae)的含量。 方法　采用LichrospherC18柱 (4 6mm× 2 5 0mm ,粒径 5 μm) ;以甲醇乙腈水 (30∶4 0∶30 )为流动相 ;流速为 0 8ml·min-1;检测波长为 2 74nm ;柱温为 2 5℃ ;进样量为 2 0 μl。结果　Pae的线性范围为 0 0 2～ 2 5 6 0mg·L-1,回归方程为 ^Y =3772 5 2 5 8X - 0 74 74 ,r =1 0 0 0 0 ,n =5 ;平均回收率为99 87% ;日内、日间变异均小于 4 %。结论　该法简便、快速 ,可用于Pae及其制剂的含量测定。     

HPLC法测定西红花康复液中丹皮酚的含量

目的 :建立西红花康复液中丹皮酚的高效液相色谱分析方法。方法 :以KomasilODS 1(4 .6mm× 2 0 0mm ,5 μm)为色谱柱 ,流动相为甲醇∶水 (5 0∶5 0 ) ,流速为 1ml·min-1,柱温 4 0℃ ,检测波长 2 74nm。结果 :线性范围为 0 .0 6 3～ 0 .378μg(r =0 .9998) ,平均加样回收率为 97.2 4 % ,RSD为 2 6 .3% (n =9)。结论 :本方法快速、简便 ,适用于本制剂的质量控制。     

HPLC法同时测定胃痛欣颗粒剂中大黄酸、大黄素、大黄酚的含量

目的建立胃痛欣颗粒剂中大黄酸、大黄素、大黄酚的含量测定方法。方法采用高效液相色谱法 ,AccusilC1 8(4 6mm× 2 5 0mm ,1 0 μm)柱 ,流动相为 :甲醇 水 冰醋酸 (80∶2 0∶1 ,V∶V∶V) ,检测波长为 2 5 4nm。结果大黄酸、大黄素、大黄酚分别在 0 0 3～ 0 4 8μg ,0 0 2 5～ 0 4 0 μg ,0 0 2 5～0 4 0 μg内与峰面积呈线性关系 ,平均回收率 (n =3 )分别为 98 3 % (RSD =1 4 3 % ) ,97 6% (RSD=1 84 ) ,98 7% (RSD =0 5 7% )。结论可用于大黄药材及其复方制剂的质量控制     

高效液相色谱法测定苍芷喷鼻液中丹皮酚、欧前胡素的含量

目的 :建立测定苍芷喷鼻液中丹皮酚、欧前胡素含量的高效液相色谱方法。方法 :色谱柱为HypersilDivisionODSC18(150mm×4 6mm ,5μm ) ,流动相为甲醇 -水 (6∶4) ,检测波长为310nm ,流速为1 0ml/min ,室温操作。结果 :丹皮酚、欧前胡素平均回收率分别为99 4 % (RSD=0 69 % )、99 9 % (RSD=2 66 % )。结论 :本方法快速、准确 ,样品处理简便易行。     

HPLC法测定牡丹皮中丹皮酚的含量

目的　建立高效液相色谱法测定牡丹皮中丹皮酚含量的方法。方法　选用C18色谱柱 ,甲醇 -水 (6 5∶35 )为流动相 ,检测波长为 2 74nm ,流速 :1 0ml·min-1。结果　在 3～ 18μg·ml-1范围内有良好的线性关系 ,平均回收率为 98 9% (n =5 ) ,RSD =1 5 %。结论　本方法简便、准确、重现性好 ,可以作为丹皮酚的质量控制方法     

超声提取法测定熊胆消炎胶囊中大黄素和大黄酚的含量

目的　建立熊胆消炎胶囊中大黄素和大黄酚的含量测定方法。方法　采用超声提取RP -HPLC法测定 ,用Shim packCLC -ODS柱 (6 0mm× 15 0mm ,5 μm) ,以甲醇 - 0 1%磷酸溶液 (85∶15 )为流动相 ,检测波长 2 5 4nm。 结果　大黄素的线性范围为 4 0 88～ 81.76ng(r=0 .9999) ,平均回收率为 99 3% ,RSD =0 93% (n =9) ;大黄酚的线性范围为 8 2 72～ 16 5 4 4ng(r =0 9999) ,平均回收率为 99 5 % ,RSD =1 86 % (n =9)。测定大黄素方法精密度RSD =0 .6 0 % (n =5 ) ,测定大黄酚RSD =0 6 5 %(n =5 )。结论　所用方法测定样品的分离效果佳 ,灵敏度高 ,重复性好 ,结果准确可靠。     

HPLC测定丹皮酚软膏（丹皮酚霜）中丹皮酚的含量

目的:采用 HPLC 法测定丹皮酚软膏(霜)中丹皮酚的含量。方法:色谱柱为 Hypersil C_(18)柱(150 mm×4.6 mm,5 μm);流动相:甲醇-水(50:50);流速1.0 mL·min~(-1);检测波长:274 nm。结果:丹皮酚进样量在0.05～0.54 μg范围内呈良好线性关系(r=0.9998),平均回收率(n=6)为98.7%,RSD 为2.0%。结论:本法准确,重现性好。     

毛细管气相色谱法测定康溃丸中丹皮酚的含量

目的 :建立直接蒸馏毛细管气相色谱法测定康溃丸中丹皮酚的含量。方法 :色谱柱HP 5 (3 0m× 0 3 2mm ,0 2 5 μm) ,N2 (99 999% ) 1mL·min-1,空气 3 5 0mL·min-1,H2 4 0mL·min-1,柱温 15 0℃ ,检测室 2 2 0℃ ,气化室 2 2 0℃ ,分流比 1∶10 0 ,尾吹气流量 3 0mL·min-1。结果 :该方法的线性范围为 0 0 80 1～ 0 9612mg·mL-1,r=1 0 0 0 0 ;加样回收率为 99 7% ,RSD为 0 86% (n=6)。结论 :本法简便 ,准确 ,灵敏度高 ,重现性好 ,可用于康溃丸中丹皮酚的含量测定     

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.