HPLC法测定心神宁胶囊中栀子苷的含量

目的建立心神宁胶囊中栀子苷含量的HPLC测定方法。方法采用高效液相色谱法,色谱柱为ODS2柱,流动相为乙腈-水(12∶88),流速1.0mL.min-1,检测波长238nm。结果该方法线性关系良好,平均加样回收率为98.4%,RSD为0.3%(n=6)。结论方法快速、简便、灵敏,分离度好,适用于心神宁胶囊的含量测定。     

HPLC法同时测定心神宁片中栀子苷和甘草苷的含量

目的:建立同时测定心神宁片中栀子苷和甘草苷含量的方法。方法:采用高效液相色谱法。色谱柱为Inertsil ODS-3,流动相为乙腈-水(梯度洗脱),流速为1.0 ml/min,柱温为25℃,检测波长为238 nm,进样量为10μl。结果:栀子苷、甘草苷质量浓度分别在16.3~407.9、7.4~185.9μg/ml范围内与各自峰面积呈良好的线性关系(r均为0.999 9);精密度、稳定性、重复性试验的RSD≤1.63%;平均加样回收率分别为99.05%、98.00%,RSD分别为1.28%、1.84%(n=9)。结论:该方法准确、灵敏、简便,可用于心神宁片中栀子苷和甘草苷的含量测定。     

高效液相色谱法测定梦宁片中栀子苷的含量

目的 :采用高效液相色谱法测定梦宁片中栀子苷含量。方法 :采用EclipseXDB C18色谱柱 (4 .6mm× 2 5 0mm ,5μm) ,以0 .2 %三乙胺水溶液 (含 0 .1%磷酸 ) 乙腈 (85∶15 )为流动相 ,检测波长为 2 4 0nm ,流速 1.0mL·min-1。结果 :栀子苷进样量在 0 .0 988μg～0 .4 94 0 μg范围内与峰面积积分值具有良好的线性关系 ,相关系数r =0 .9995 (n =5 ) ,回收率为97.91% (n =5 )。结论 :本方法操作简便 ,精密度好 ,结果准确可靠。     

肾宁片质量标准研究

目的:建立肾宁片的质量标准。方法:采用薄层色谱(TLC)法对肾宁片中益母草、大黄、栀子、黄柏进行定性鉴别;采用高效液相色谱法测定栀子苷、芍药苷的含量。结果:TLC可鉴别出益母草、大黄、栀子、黄柏相对应的斑点。栀子苷、芍药苷的进样量分别在0.032 2～0.386 4μg(r=0.999 9)、0.041～0.492μg(r=0.999 9)范围内与各自峰面积积分值呈良好的线性关系;二者平均回收率分别为101.09%、100.08%,RSD分别为0.54%(n=6)、1.28%(n=6)。结论:所建标准可用于肾宁片的质量控制。     

柱层析-高效液相色谱法测定乳增宁片中淫羊藿苷含量

目的 :建立乳增宁片中淫羊藿苷含量新的测定方法。方法 :采用聚酰胺柱层析 -高效液相色谱法 ,色谱柱为C18 柱 ,流动相为乙腈 -水 (30∶70) ,检测波长为270nm。结果 :淫羊藿苷在10～18μg/ml检测浓度范围内线性关系良好 (r=0 9995) ,平均回收率为94 6 % (RSD=1 95 % ,n=6)。结论 :本法能有效消除乳增宁片中其它成分对含量测定的干扰 ,且简便、准确、重现性好。     

高效液相色谱法测定牛黄上清片中栀子苷的含量

目的：建立牛黄上清片中栀子苷的含量测定方法。方法：采用高效液相色谱法测定牛黄上清片中栀子苷的含量。色谱柱：DikmaKromasil C18柱（250×4．6mm,5μm）;流动相：乙腈-水（15：85）;检测波长：238nm;柱温：25℃;流速：1．0ml/min;进样量：10．0μl。结果：栀子苷在0．4204～4．204μg范围内有良好的线性关系（r=0．9998）,平均回收率为98．03％,相对标准差（RSD）为1．15％（n=6）。测得牛黄上清片中栀子苷的平均含量为2．3848mg／g。结论：该方法简便易行、快速准确,具有良好的重复性和回收率,可作为牛黄上清片中栀子苷的定量分析方法。     

HPLC测定复方鸡骨草胶囊中栀子苷含量

目的:建立复方鸡骨草胶囊(鸡骨草、栀子、枸杞子、白芍)中栀子苷含量测定方法.方法:采用HPLC,以CLC-ODS柱为固定相,甲醇-0.1%磷酸溶液(22:78)为流动相,检测波长为240 nm.结果:栀子苷在(00248-0.148 8)mg/ml(r=0.999 9)范围内呈良好的线性关系,平均加样回收率栀子苷99.52%、RSD=1.18%(n=6).结论:含量测定方法简便准确,重复性好,可用于控制复方鸡骨草胶囊的质量.     

HPLC法测定肝宁丸中栀子苷的含量

目的:应用高效液相色谱法对肝宁丸中栀子苷进行含量测定.方法:选用依利特Hypersil C18分析柱(150 mm×4.6 mm,5μm),乙腈-水(11:89)为流动相,检测波长为238 nm,流速1.0 ml · min-1.结果:栀子苷在0.016 7～0.333 2 mg·ml-1具有良好的线性关系,r=1.000 0,平均回收率为96.10%,RSD为0.96%.结论:本试验所确定的质量分析方法稳定可靠,可作为肝宁丸中栀子苷的含量测定方法.     

HPLC法测定茵栀黄软胶囊中黄芩苷、栀子苷和绿原酸的含量

目的测定茵栀黄软胶囊中的 3种有效成分 ,黄芩苷、栀子苷、绿原酸的含量。方法HPLC法 ,Irregular HC18(2 5 0 . 0mm× 4 6mm ,10 μm)色谱柱。黄芩苷流动相 :甲醇 水 磷酸 (V∶V∶V =4 7. 0∶5 .3 0∶0. 2 ) ,流速 :1 0mL·min-1,检测波长 :2 80nm ;栀子苷流动相 :乙睛 水 (V∶V =15∶85 ) ,流速 :1 0mL·min-1,检测波长 :2 38nm ;绿原酸流动相 :乙睛 磷酸溶液 (w =0 . 4 % )(V∶V =13∶87) ,流速 :1 0mL·min-1,检测波长 :32 7nm。结果黄芩苷在 2 7 5～ 137 5mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =6 4. 83× 10 4ρ - 1 6. 96× 10 .5 ,r =0 . 9998,平均回收率为 99 4 6 % (RSD =1 0 1% ) ;栀子苷在 16 .5～ 82 . 5mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =8 794× 10 .5ρ - 4 . 116× 10 2 ,r =0 . 9999,平均回收率为 10 0 . 37% (RSD =1 4 .0 % ) ;绿原酸在 2 4～ 12 0mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =2 4 88× 10 4ρ - 9 2 4 4× 10 4,r =0 9999,平均回收率为 99 38%(RSD =1. 89% )。结论测定方法可用于茵栀黄软胶囊的质量控制。     

高效液相色谱-蒸发光散射检测法测定因宁片中黄芪甲苷的含量

目的建立因宁片中黄芪甲苷的含量测定方法。方法采用高效液相色谱 蒸发光散射检测法测定。结果黄芪甲苷在0.6～7.5 μg与峰面积积分值呈良好的线性关系( r = 0.9996, n = 5) ，平均回收率98.0%。结论该方法测定因宁片中黄芪甲苷的含量可行。     

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.