双波长RP-HPLC同时测定黄连上清片中栀子苷和黄芩苷的含量

目的建立同时测定黄连上清片中栀子苷、黄芩苷含量的方法。方法采用双波长高效液相色谱法,色谱柱为Hibor C18柱（4.6 mm×150 mm,5μm）,流动相为乙腈-0.2%磷酸水溶液,梯度洗脱;栀子苷和黄芩苷检测波长分别为240 nm和278 nm;柱温为30℃。结果栀子苷和黄芩苷进样量分别在0.16～0.8μg（r=0.999 7）和0.24～1.2μg（r=0.999 8）内线性关系良好;平均加样回收率分别为95.7%和96.1%,RSD分别为2.63%和1.37%。结论方法简便、准确、重复性好,适用于黄连上清片中栀子苷和黄芩苷的含量测定。     

HPLC法测定牛黄上清片中黄芩苷的含量

目的:建立以高效液相色谱法测定牛黄上清片中黄芩苷含量的方法。方法:色谱柱为ODS(C18),流动相为甲醇-水-磷酸(40∶60∶0.2),流速为0.8ml·min-1,检测波长为280nm,柱温为室温。结果:黄芩苷进样量在0.06～0.54μg范围内线性关系良好(r=0.9995),平均加样回收率为98.58%(RSD=1.49%)。结论:该方法简便、快速、准确、重现性好,可用于牛黄上清片中黄芩苷的含量测定。     

高效液相色谱法同时测定痔特佳片中柚皮苷和黄芩苷的含量

目的建立HPLC法同时测定痔特佳片中柚皮苷和黄芩苷的含量。方法采用Hypersil ODS2(4.6mm×250mm,5μm)色谱柱;流动相:乙腈-水(20∶80)(用磷酸调节pH值至3.0);流速:1.0mL.min-1;检测波长:283nm;柱温:35℃。结果柚皮苷进样量在0.0540μg~0.540μg(r=0.9998),黄芩苷进样量在0.0626μg~0.626μg(r=0.9999),与峰面积线性关系良好;柚皮苷平均回收率为99.28%,RSD为1.45%(n=9);黄芩苷平均回收率为100.33%,RSD为1.27%(n=9)。结论该方法简便,快速,结果可靠,可用于痔特佳片的质量控制。     

HPLC法同时测定小儿导赤片中栀子苷和大黄酚含量

目的 建立测定小儿导赤片中栀子苷和大黄酚的含量.方法 采用高效液相色谱法,以乙腈为流动相A,0.1％磷酸溶液为流动相B,梯度洗脱;检测波长为238nm(栀子苷),254nm(大黄酚),柱温:40℃;流速:1.0mL·min-1;进样量:101μL.结果 栀子苷在6.01μg～120.20μg范围内线性良好(r =0.9999,n=5),大黄酚在1.234μg～24.68μg范围内线性良好(r=0.9999,n=5),平均回收率分别为99.7％和99.7％,RSD分别为0.8％和1.0％.结论 本方法可用于测定小儿导赤片中栀子苷和大黄酚含量.     

高效液相色谱法测定山丹酮缓释片中牡荆苷和金丝桃苷的含量

建立高效液相色谱法测定山丹酮缓释片中牡荆苷和金丝桃苷的含量.色谱柱Lichrospher C18(5μm, 250mm×4.6mm), 流动相:甲醇-水-冰醋酸(50∶50∶1);检测波长:340 nm;牡荆苷和金丝桃苷的线性范围分别为:0.73～3.66μg(r=0.9999)和0.63～3.16μg (r=0.9998);平均回收率分别为:100.03%,RSD=1.17% (n=5)和99.81%,RSD=0.36%(n=5).本法操作简单,快速,准确,可行.     

高效液相色谱法测定耳聋丸中栀子苷和黄芩苷含量

目的 建立一种同时测定耳聋丸中栀子苷和黄芩苷含量的高效液相色谱法.方法 采用Agilent Extend-C18柱(250mm×4.6mm,5μm),以甲醇-0.5%冰醋酸溶液为流动相,梯度洗脱;流速0.8 mL/min;检测波长240 nm;进样量10μL;柱温:室温.结果 栀子苷和黄芩苷与其相邻杂质峰能完全分离,栀子苷进样量在0.0544~0.5440μg,内与峰面积具有良好的线性关系,r=0.9997(n=5);黄芩苷进样量在0.313 6~3.1360 μg内与峰面积具有良好的线性关系,r=1.000 0(n=5);栀子苷和黄芩苷平均回收率分别为97.38%和97.86%.RSD分另q为1.14%和0.62%(n=6).结论 所用方法简便、快速、准确,一种方法能同时测定两种成分,可用于耳聋丸的质量控制.     

HPLC 法测定女金片中橙皮苷和黄芩苷的含量

目的:建立测定女金片中橙皮苷和黄芩苷含量的HPLC法.方法:色谱柱:Eclipse XDB-C18柱(250 mm×4.6 mm,5μm),流动相:乙腈-0.2%磷酸(20:80),检测波长:280 nm,流速:1.0 ml·min-1.结果:橙皮苷进样量在0.022～0.220μg范围内与峰面积呈良好的线性关系,r=0.999 5,平均回收率为98.63%,RSD为0.69%(n=6);黄芩苷进样量在0.046～0.460μg范围内与峰面积呈良好的线性关系,r=1.000 0,平均回收率为98.90%,RSD为0.49%(n=6).结论:该方法快速简便,专属性强,结果准确,适用于女金片中的橙皮苷和黄芩苷的含量测定.     

HPLC法同时测定茵苓祛湿汤中绿原酸、栀子苷的含量

目的:建立同时测定茵苓祛湿汤中绿原酸、栀子苷含量的方法。方法:采用高效液相色谱法。色谱柱为KromasilC18(250mm×4.6mm,5μm),流动相为乙腈-0.4%磷酸(13:87),流速为1.0mL·min-1,双波长检测:绿原酸327nm、栀子苷238nm。结果:绿原酸进样量在0.1544～1.2352μg范围内与峰面积积分值呈良好线性关系(r=0.9997),平均回收率为99.9%,RSD=0.54%(n=6);栀子苷进样量在0.3632～2.9056μg范围内与峰面积积分值呈良好线性关系(r=0.9999),平均回收率为100.0%,RSD=0.51%(n=6)。结论:本方法简单、快捷、准确,适用于测定茵苓祛湿汤中绿原酸、栀子苷的含量。     

HPLC法同时测定栀子金花丸中栀子苷和黄岑苷的含量

目的建立HPLC法同时测定栀子金花丸中栀子苷和黄芩苷的含量测定方法。方法采用AgilentTC-C18色谱柱;甲醇-0.5%冰醋酸溶液为流动相,梯度洗脱;流速为0.8mL.min-1;检测波长为239nm。结果栀子苷和黄芩苷与其相邻杂质峰能完全分离,栀子苷在9.760～97.60μg.mL-1浓度范围内线性关系良好,r=0.9999;黄芩苷在10.42～104.2μg.mL-1浓度范围内线性关系良好,r=0.9999。栀子苷和黄芩苷平均回收率分别为100.56%、101.15%,RSD为2.57%和2.82%。结论本方法简便、准确、重复性好,能排除其他成分的干扰,可用于该制剂的质量控制的评价。     

HPLC法测定复肾宁片中栀子苷的含量

目的:用高效液相色谱法测定复肾宁片中栀子苷的含量。方法:采用Agilent C_(18)(250 mm×4.6 mm,5μm)色谱柱,以乙腈-水(10:90)为流动相,流速:1.0ml·min~(-1),检测波长为238 nm。结果:栀子苷进样量在0.1446～1.446μg(r= 0.9999)范围内,与峰面积呈良好的线性关系。栀子苷的平均回收率为100.9%,RSD=1.1%(n=6)。结论:本方法简便可靠,专属性强,重现性好,可用于该制剂的质量控制。     

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.

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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.