HPLC法测定当归苦参丸中阿魏酸的含量

目的建立当归苦参丸中阿魏酸的高效液相色谱含量测定方法。方法采用C18柱(250mm×4.6mm,5μm),以乙腈-0.085%磷酸(17∶83)为流动相,流速为1mL·min-1,柱温为30℃,检测波长为316nm。结果线性范围为0.02856～0.14280μg,精密度试验RSD为0.9%,回收率为99.9%,RSD为2.2%(n=5)。结论方法快速、简便、准确、重现性较好,结果可靠,可为当归苦参丸的质量评价提供依据。     

高效液相色谱法测定当归苦参丸中阿魏酸的含量

目的:建立HPLC法测定当归苦参丸中阿魏酸的含量。方法:采用Kromasil C18柱(250mm×4.6mm,5μm)色谱柱;流动相为0.085%磷酸溶液(以10%三乙胺溶液调pH3.0)-乙腈(83∶17);检测波长为316nm,流速为1.0mL.min-1。结果:阿魏酸的线性范围为2.01~40.2mg.L-1,精密度试验RSD为1.1%,重复性试验RSD为1.0%,平均回收率99.4%,RSD为1.7%(n=9)。结论:该方法简便、可靠、准确,可用于该制剂的质量控制。     

高效液相色谱法测定当归养血丸中阿魏酸含量

目的建立当归养血丸中阿魏酸含量测定方法。方法采用高效液相色谱法。色谱条件：色谱柱为HypersilC18柱（250mm×4.6mm,5μm）;流动相：甲醇-1%冰乙酸溶液（25∶75）;柱温：25°C;流速：1.0ml/min;检测波长为320nm;理论塔板数按阿魏酸峰计算不低于3000。结果阿魏酸在0.03～0.48μg范围内线性关系良好,r=0.9997。阿魏酸平均回收率为98.90%,RSD为0.94%。结论该方法操作简单、准确、重复性好,可用于当归养血丸的质量控制。     

当归补血微丸的制备及其质量控制

目的制备当归补血微丸并建立其质量控制方法。方法以挤出滚圆法制备当归补血微丸,考察微丸的粉体学性质和溶散时限,并采用高效液相色谱法测定微丸中阿魏酸的含量。结果所制微丸圆整度、流动性好,溶散时限合格。阿魏酸进样量在0.03438μg~1.146μg范围内线性关系良好(r=0.9998),平均回收率为97.0%(RSD=0.664%)。结论该制剂制备方法可行;所建立的含量测定方法准确、灵敏、稳定性好,可用于该制剂的质量控制。     

HPLC法测定当归片中阿魏酸的含量

目的:测定当归片中阿魏酸含量.方法:采用十八烷基硅烷键合硅胶柱;流动相为乙腈-水-冰醋酸(21:78:1),检测波长为322nm;流速为1.0ml/min.结果:阿魏酸平均回收率为98.3%,RSD为0.9%(n=5).结论:本法操作简便,结果准确,可以作为当归片的质量控制方法.     

HPLC法测定养血当归糖浆中阿魏酸和芍药苷的含量

建立HPLC法同时测定养血当归糖浆中阿魏酸和芍药苷的含量.采用Hypersil ODS C18色谱柱,流动相:乙腈-0.1%磷酸溶液(10:90);流速:1.0mL·min-1,检测波长:230nm,柱温:25℃.阿魏酸浓度的线性范围0.0004024～0.004828mg·mL-1,r=0.9994;芍药苷浓度的线性范围0.007232～0.08678mg·mL-1,r=0.9994;平均回收率阿魏酸为100.35%,RSD为1.64%;芍药苷为98.15%,RSD为1.62%.该法简便,结果可靠,可有效地用于养血当归糖浆的质量控制.     

RP-HPLC法测定当归四逆颗粒中阿魏酸的含量

目的　建立RP HPLC测定当归四逆颗粒中阿魏酸的定量方法。方法　以反相高效液相法测定阿魏酸的含量。固定相 :ShimpackCLC_ODS(150mm× 6mm) ;流动相 :含 0 2 %甲醇的乙腈 含 0 1%磷酸和 0 1%三乙胺水溶液 (2 0∶80 ) ;检测波长 3 2 4nm。结果　阿魏酸在 1 2 4～ 2 4 80 μg/ml范围内线性良好 (r =0 9998) ,平均加样回收率为 98 7% ,RSD为 1 7%。 结论　定量方法简便 ,准确 ,能有效地控制当归四逆颗粒剂的质量     

HPLC法测定当归片中阿魏酸的含量

目的:建立高效液相色谱法测定当归片的含量。方法:色谱柱为Zorbaxl C18,流动相为乙腈-0.085%磷酸溶液(17∶83),检测波长为316 nm,流速为1.0 mL﹒min-1。结果:阿魏酸进样量在9.724～58.344μg.mL-1范围内线性关系良好(r=0.9999,n=6)。阿魏酸的平均回收率为99.7%,RSD为1.7%(n=6)。结论:本法简便、准确,重现性好,可作为当归片的质量控制方法。     

高效液相色谱法测定中药当归中阿魏酸的含量

目的测定中药当归中阿魏酸的含量。方法采用HPLC法,Sucleosil C18柱(250mm×4.6mm,7μm),以乙腈-0.1%冰醋酸溶液(17∶83)为流动相,流速为1m.lm in-1,检测波长为316nm,柱温35℃。结果阿魏酸在0.03636~0.21816μg范围内,线性关系良好(r=0.9999)。平均回收率为103.04%(n=5),RSD为1.68%。结论本法灵敏、准确,简便易行,重复性好,可用于中药当归药材及饮片的质量控制。     

正交设计优选当归苦参丸仿生提取工艺

目的:探索当归苦参丸的新型仿生提取方法。方法:采用液-液连续萃取法,用酸水、碱水模拟胃肠环境,以正辛醇模拟生物膜结构,以阿魏酸和苦参碱提取效率为考察指标,采用L₈（3⁴）正交试验法,探讨酸（碱）水体积、pH及蒸馏时间对阿魏酸、苦参碱提取的影响。结果:模拟胃环境仿生提取最佳工艺为A₁B₁D₃,即酸水4倍量,pH为1,蒸馏时间6 h;模拟肠环境仿生提取最佳工艺为A₁B₃D₃,即碱水4倍量,pH为9,蒸馏时间6 h。结论:仿生提取法提取阿魏酸、苦参碱简便、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.