HPLC法测定注射用络通冻干粉中芍药苷的含量

目的建立了注射用络通冻干粉中芍药苷含量测定的H PLC法。方法用W ater的C18反相色谱柱(4.6m m×150m m,5μm),以甲醇:0.03m ol/L的磷酸二氢钾:5%的庚烷磺酸钠(60:30:10)为流动相,流速为1.0m L·m in-1,用二极管阵列检测器检测,检测波长230nm,柱温30℃。结果方法的线性范围为:87.8～1756μg·m L-1(r=0.9997),精密度RSD为0.26%(n=7),重现性RSD为0.84%(n=5),芍药苷的平均回收率为99.19%,RSD为0.76%(n=6)。结论方法快速、简便,结果准确、可靠,可用于注射用络通冻干粉中芍药苷的含量测定。     

HPLC法测定炎痢净片中芍药苷的含量及溶出度

目的:建立测定炎痢净片中芍药苷的含量及溶出度的方法.方法:采用SinoChron ODS-BP色谱柱(250 mm×4.6 mm,5 μm),流动相为乙腈-0.1%磷酸(14:86),流速1.0 ml·min-1,检测波长285 nm,柱温35℃.结果:芍药苷在0.41~41.20 μg·ml-1范围内线性关系良好(r=0.999 9),平均回收率为99.6%(RSD=1.80%,n=6).结论:该方法简便、可靠,可作为炎痢净片中芍药苷的含量及溶出度测定.     

RP-HPLC法测定痛泻要方中芍药苷的含量

目的 建立反相高效液相色谱法测定痛泻要方中芍药苷的含量.方法 采用Kromasil C18色谱柱(250 mm×4.6mm,5μm);以甲醇-水(25∶75)为流动相;检测波长为230nm;流速为1.0ml·min-1;柱温30℃.结果 芍药苷在14.24～142.4μg·mL-1范围内呈良好线性关系(r=0.99993,n=7);平均回收率为100.07%,RSD为1.96%(n=6).结论 该方法 测定结果 灵敏、准确、重现性好,可用于痛泻要方中芍药苷的含量测定.     

HPLC法同时测定养血清脑胶囊中芍药苷和阿魏酸的含量

目的建立同时测定养血清脑胶囊中芍药苷和阿魏酸含量的方法。方法采用HPLC法。色谱柱为Diamonsil C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-体积分数0.085%磷酸溶液,梯度洗脱,流速为1.0 mL·min-1,检测波长为240 nm,柱温为30℃。结果芍药苷质量浓度在4.96¹9.84 mg·L-1内与峰面积呈良好的线性关系(r=0.999 6),平均回收率为97.1%(RSD=1.9%,n=6);阿魏酸质量浓度在2.5219.84 mg·L-1内与峰面积呈良好的线性关系(r=0.999 6),平均回收率为97.1%(RSD=1.9%,n=6);阿魏酸质量浓度在2.52¹0.08 mg·L-1内与峰面积呈良好的线性关系(r=0.999 0),平均回收率为100.1%(RSD=2.8%,n=6)。结论建立的方法简便、准确、重复性好,可用于养血清脑胶囊的质量控制。     

HPLC法测定同仁乌鸡白凤丸中芍药苷和丹参素的含量

目的:建立测定同仁乌鸡白凤丸中芍药苷和丹参素含量的方法。方法:采用 C_(18)柱(250mm×4.6 mm,5 μm)测定芍药苷的含量,流动相为甲醇-水(30:70),流速1 mL·min~(-1),检测波长232 nm;采用 C_(18)柱(250 mm×4,6 mm,5μm)测定丹参素的含量,流动相为甲醇-0.5%醋酸(8:92),流速1 mL·min~(-1),检测波长281 nm。结果:芍药苷的线性范围为0.0119～0.0595 mg·mL~(-1)(r=0.9993),平均同收率(n=6)为100.1%(RSD 为2.5%);丹参素的线性范同为0.0248～0.1240 mg·mL~(-1)(r=0.9993),平均回收率(n=6)为95.5%(RSD 为1.6%)。结论:本方法操作简便,结果准确可靠,重复性好,可用于同仁乌鸡白凤丸的质量控制。     

HPLC法测定消乳癖颗粒中芍药苷的含量

目的:建立高效液相色谱法测定消乳癣颗粒中芍药苷的含量.方法:色谱柱;Kromasil C18柱(250 mm×4.6 mm,5μm),流动相:乙腈-水( 13∶87),检测波长:230 nm,柱温为30℃,流速为1.0 ml ·min-1.结果:芍药苷在0.228～2.280μg范围内线性关系良好,r =0.999 9,平均回收率为99.9％,RSD=1.87％(n=6).结论:该方法简便,结果准确,可用于消乳癖颗粒中芍药苷的含量测定.     

HPLC法测定赤牡泡腾片中芍药苷的含量

目的:建立高效液相色谱法测定赤牡泡腾片中芍药苷含量的方法.方法:采用Zobax Eclipse XDB-C18(250 mm×4.6 mm,5μm)色谱柱,乙腈-水(11:89)为流动相,流速:1.0 ml·min-1,柱温:30℃,检测波长230 nm.结果:芍药苷的线性范围为5.06~80.96 μg·ml-1(r=0.999 9).平均回收率为98.30%(RSD=0.91%,n=6).结论:本方法准确、简便、快速,能用于测定赤牡泡腾片中芍药苷的含量.     

高效液相色谱法测定白芍药材中芍药苷和芍药内酯苷的含量

目的:建立高效液相色谱法测定白芍药材中芍药苷和芍药内酯苷含量的方法.方法:采用高效液相色谱法,色谱柱:Kromasil ODS2 (4.6 mm×250 mm,5 μm),流动相:甲醇-0.1％磷酸溶液(用1％氢氧化钠溶液调节pH值至4.2)(34:66);流速:1.0 mL·min-1,检测波长:230 nm.结果:芍药内酯苷在0.018～0.576 μg范围内呈线性关系(r=0.9999),芍药苷在0.028～0.896μg范围内呈线性关系(r=0.9999);芍药内酯苷加样回收率为98.18％(n=6),RSD值小于2％,芍药苷加样回收率为98.26％(n=6),RSD值小于2％.结论:本研究所建方法灵敏、简便,能同时准确测定白芍药材中芍药苷和芍药内酯苷的含量.     

HPLC法测定摩罗丹中芍药苷的含量

目的建立摩罗丹的质量控制方法。方法采用Agi-lent C18(150 mm×4.6 mm,5μm)色谱柱,以乙腈-0.05%磷酸二氢钾溶液(14∶86)为流动相,检测波长为230 nm;柱温:30℃;流速:1.0 m l·m in-1;测定摩罗丹中芍药苷的含量。结果芍药苷的线性范围为0.0872~0.872 mg·L-1(r=0.9996,n=5),平均回收率为98.6%(RSD=0.9%,n=6)。结论该方法简便、准确、专属性强,可有效控制摩罗丹的质量。     

HPLC法测定肝血瘤康糖浆中芍药苷的含量

目的:建立HPLC法测定肝血瘤康糖浆中芍药苷含量的方法.方法:采用DIONEX C18色谱柱(250 mm×4.6 mm,5 μm),甲醇-0.05mol·L-1磷酸二氢钾溶液(38:62)为流动相,流速:1.0ml·min-1,柱温:30℃,检测波长:230 nm.结果:芍药苷在0.12～5.99μg(r=0.999 8)范围内呈良好的线性关系,平均回收率为100.4%(RSD=0.8%,n=6).结论:本方法灵敏、简便、准确,可用于肝血瘤康糖浆中芍药苷的含量控制.     

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.