HPLC法测定利通淋胶囊中总黄酮醇苷的含量

目的建立HPLC法测定利通淋胶囊中总黄酮醇苷含量。方法采用Kromasil C18(4.6×250mm,5μm)色谱柱;流动相:甲醇-0.4%磷酸溶液(55∶45);流速:1.0mL.min-1;测定检测波长为360nm。结果槲皮素在浓度4.067μg·mL-1~40.67μg·mL-1范围内线性关系良好(r=0.9998);山奈酚在浓度0.871μg·mL-1~8.71μg·mL-1范围内线性关系良好(r=0.9998);异鼠李素在浓度0.616μg·mL-1~6.16μg.mL-1范围内线性关系良好(r=0.9996)。结论本方法简便、准确、专属性强,可测定利通淋胶囊中总黄酮醇苷的含量。     

HPLC法快速测定银杏叶中银杏总黄酮醇苷含量

目的建立银杏叶中特征性成分总黄酮醇苷的快速含量分析方法,比较不同的采集地总黄酮醇苷含量差异。方法采用Alltima C18色谱柱(5μm,4.6×150mm);流动相为甲醇-0.4%磷酸(50∶50);检测波长为360nm;流速为1.0mL/min;柱温为30℃。结果Q在0.06～0.60μg范围内线性关系良好(r=0.9998);K在0.06～0.06μg范围内线性关系良好(r=0.9998);I在0.04～0.40μg范围内线性关系良好(r=0.9999)。平均加样回收率为97.6%(n=6),RSD为1.22%,银杏总黄酮醇苷的含量为0.4857%～0.8869%。结论不同产地银杏叶中总黄酮醇苷含量差异较大,该方法准确、简便,重现性好,为银杏叶质量评价提供简便快捷的方法。     

银杏绞股蓝胶囊的质量控制

目的:制定银杏绞股蓝胶囊的质量控制方法。方法:采用HPLC法测定银杏绞股蓝胶囊中含有的银杏总黄酮醇苷和人参皂苷Rb₁的含量;通过急性毒性实验验证银杏绞股蓝胶囊的安全用量。结果:HPLC法测得总黄酮醇苷中槲皮素、山柰素、异鼠李素进样量分别在0.06～0.75μg（r=0.9999）、0.06～0.75μg（r=0.9998）、0.04～0.50μg（r=0.9998）范围内与峰面积呈良好的线性关系,平均加样回收率分别为99.12%,98.96%,98.66%;HPLC梯度洗脱法测定绞股蓝总苷中人参皂苷Rb₁的含量,Rb1在进样量0.4～8.0μg（r=0.9996）范围内与峰面积呈良好的线性关系,平均加样回收率分别为96.98%;银杏绞股蓝胶囊口服途径的小鼠LD₅₀大于3 200mg·kg^-1,表明在临床常用剂量下是安全的。结论:建立的HPLC方法简便可行,准确可靠,可用于该胶囊的质量控制。     

HPLC法测定骨刺消痛胶囊中白芷的含量

目的建立骨刺消痛胶囊中白芷的含量测定方法。方法采用HPLC法对骨刺消痛胶囊中白芷(以欧前胡素和异欧前胡素计)的含量进行测定。结果欧前胡素在6.0～60.0μg·mL-1范围内呈良好的线性关系,r=0.9998,平均回收率为93.6%,RSD=2.48%(n=6);异欧前胡素在4.0～40.0μg·mL-1范围内呈良好的线性关系,r=0.9998,平均回收率为90.4%,RSD=1.51%(n=6)。结论该方法简便、可靠、重复性好,可用于骨刺消痛胶囊中白芷的含量测定。     

HPLC法测定地西他滨中L-异构体和α-异构体含量

目的 建立高效液相法对地西他滨中L-异构体和α-异构体进行拆分并检测其中异构体含量.方法 色谱柱采用CHIRACPAK-ADH手性柱(250mm ×4.6mm,5μm);流动相:无水乙醇一正己烷(50∶50);流速:0.5mL·min-1;检测波长:244nm;选样量:20μL.结果 本法对L-异构体和α-异构体的分离度为2.42,地西他滨浓度在0.395～4.02μg·mL-1范围内呈良好的线性关系(r =0.9999),L-异构体浓度在0.419 ～4.04μg·mL-1范围内呈良好的线性关系(r=0.9997),α-异构体浓度在0.419 ～4.02μg·mL-1范围内呈良好的线性关系(r =0.9998),检测限分别为5.10ng和5.08ng,平均回收率分别为98.47％和99.22％.结论 该方法操作简便,分离效果好,可用于地西他滨中异构体的含量测定.     

HPLC法同时测定通宣理肺丸中柚皮苷、橙皮苷及黄芩苷的含量

目的建立一种高效液相色谱法同时测定通宣理肺丸中柚皮苷、橙皮苷及黄芩苷的含量。方法采用高效液相色谱法,以BDSC18柱(250mm×4.6mm,5μm)为色谱柱;流动相:乙腈-0.1%磷酸溶液(20∶80);流速1.0mL.min-1;检测波长:280nm。结果柚皮苷、橙皮苷、黄芩苷分别在10.04~100.4μg·mL-1(r=0.9998)、12.9~129μg·mL-1(r=0.9998)、17.44~174.4μg·mL-1(r=0.9997)范围内浓度与峰面积呈良好的线性关系;平均回收率分别为98.56%(RSD=1.30%)、99.53%(RSD=0.92%)、99.16%(RSD=1.32%)。结论该方法简便、准确,可作为该制剂的含量测定方法。     

HPLC法同时测定肿痛安胶囊中5种成分的含量

目的建立同时测定肿痛安胶囊中:天麻素、升麻素苷、5-O-甲基维斯阿米醇苷、欧前胡素和异欧前胡素含量的HPLC法。方法色谱柱:Phenomenex Luna C_(18)柱(250mm×4.6mm,5μm);流速:1.0mL·min~(-1);柱温:25℃;流动相:甲醇-水梯度洗脱;检测波长:230nm;进样量:5μL。结果天麻素质量浓度在12.46～199.30μg·mL~(-1)范围内线性关系良好,r_1=0.999 5,平均回收率为101.2%,RSD值为1.6%(n=6);升麻素苷质量浓度在12.07～193.20μg·mL~(-1)范围内线性关系良好,r_2=0.999 7,平均回收率为100.1%,RSD值为1.8%(n=6);5-O-甲基维斯阿米醇苷质量浓度在8.12～129.90μg·mL~(-1)范围内线性关系良好,r_3=0.999 8,平均回收率为99.1%,RSD值为1.7%(n=6);欧前胡素质量浓度在12.52～200.40μg·mL~(-1)范围内线性关系良好,r_4=0.999 6,平均回收率为98.6%,RSD值为1.4%(n=6);异欧前胡素质量浓度在12.65～202.40μg·mL~(-1)范围内线性关系良好,r_5=0.999 6,平均回收率为99.0%,RSD值为0.7%(n=6)。结论该方法简单、准确,可同时测定5种成分的含量,可用于肿痛安胶囊的质量控制。     

心脑舒通胶囊中总黄酮醇苷的含量测定

目的建立心脑舒通胶囊中总黄酮醇苷的含量测定方法。方法采用HPLC法,色谱柱为C18(250mm×4.6mm,5μm)柱,以甲醇-4g.L-1磷酸溶液(50∶50)为流动相,检测波长为360nm。结果槲皮素?山柰素和异鼠李素进样量分别在0.0511～0.5110(r=0.9998),0.03072～0.3072(r=0.9996)和0.022432～0.11216μg(r=0.9997)范围内呈良好的线性关系;平均加样回收率分别为97.9%,99.79%和98.01%。RSD分别为0.92%,1.29%和1.65%(n=6)。结论方法操作简便,重复性好,可用于心脑舒通胶囊中总黄酮醇苷的含量测定。     

HPLC波长切换联合梯度洗脱法同时测定脑灵素胶囊中6个成分的含量

目的建立HPLC波长切换联合梯度洗脱法同时测定脑灵素胶囊中远志?酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、淫羊藿苷、宝藿苷Ⅰ和五味子醇甲的含量。方法采用Spurisil C18色谱柱(250mm×4.6 mm,5μm);流动相为乙腈-0.1%甲酸溶液,梯度洗脱;检测波长分别为320 nm、210 nm、270 nm和250 nm;体积流量为0.9 mL·min-1;柱温为35℃。结果远志?酮Ⅲ、3,6’-二芥子酰基蔗糖、细叶远志皂苷、淫羊藿苷、宝藿苷Ⅰ、五味子醇甲分别在1.18～29.50μg·m L-1(r=0.9996)、3.26～81.50μg·mL-1(r=0.9998)、4.09～102.25μg·mL-1(r=0.9993)、4.66～116.50μg·m L-1(r=0.9999)、2.57～64.25μg·mL-1(r=0.9995)、4.89～122.25μg·mL-1(r=0.9997)内与峰面积线性关系良好,平均回收率分别为97.0%、98.5%、99.2%、98.1%、97.4%和100.0%,RSD分别为1.5%、0.78%、1.2%、1.4%、1.3%和0.66%,10个批次脑灵素胶囊中远志?酮Ⅲ、3,6’-二芥子酰基蔗糖、细叶远志皂苷、淫羊藿苷、宝藿苷Ⅰ和五味子醇甲含量分别为0.237～0.294、0.610～0.753、0.997～1.208、1.099～1.427、0.569～0.728、1.192～1.481 mg·g-1。结论该方法简便、准确、重复性好,可用于脑灵素胶囊中6个成分的同时测定,为脑灵素胶囊的质量评价提供依据。     

RP-HPLC法测定气血双生合剂中淫羊藿苷、蛇床子素、五味子甲素与五味子乙素的含量

目的:建立高效液相色谱法测定气血双生合剂中淫羊藿苷、蛇床子素、五味子甲素、五味子乙素含量的方法.方法:Ultimate XB-C18柱(4.6mm×150 mm,5μm);流速:1.0mL·min-1;柱温:30℃;流动相:乙腈-水梯度洗脱;并切换检测波长;进样量:5μL.结果:淫羊藿苷在浓度为5.015～80.24μg·mL-1时线性关系良好,r=0.9999,平均回收率为100.2%,RSD为1.3%(n=6);蛇床子素在浓度为2.750～44.00μg·mL-1时线性关系良好,r=0.9997,平均回收率为100.40%,RSD为1.7%(n=6);五味子甲素在浓度为5.320～85.12μg·mL-1时线性关系良好,r=0.9997,平均回收率为101.2%,RSD为1.2%(n=6);五味子乙素在浓度为2.810～44.96μg·mL-1时线性关系良好,r=0.9996,平均回收率为101.9%,RSD为1.6%(n=6).结论:该方法简单、准确,能同时测定几种有效成分的含量,可作为气血双生合剂的质量控制.     

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.

---

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.     

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.     

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.     

Alzheimer’s disease – current trends in basic and clinical research. Highlights from the 16th ECNP

Advances in the molecular biological knowledge of neuronal nicotinic acetylcholine receptors (nAChRs) have led to a growing interest by the pharmaceutical industry in the development of novel compounds that selectively modulate nAChR function. The ability of (-)-nicotine, an activator of nAChRs, to enhance attentional aspects of cognition in animals and humans, to exert neuroprotective and anxiolytic-like effects, and presumably to mediate the negative correlation between smoking and Alzheimer's (and Parkinson's) Disease, has focused interest on the potential therapeutic utility of modulators of nAChR function for treatment of some of the deficits associated with these progressive, neurodegenerative conditions. Numerous compounds are known which activate nAChRs and which might serve as lead compounds toward the development of such agents. The pharmacologic diversity of neuronal nAChR subtypes suggests the possibility of developing selective compounds which would have more favourable side-effect profiles than existing agents. This broader class of agents, collectively called cholinergic channel modulators (ChCMs), is anticipated to encompass compounds which would have more favourable side-effect profiles than existing agents, which generally exhibit low selectivity. This selectivity may be achieved by preferentially activating some subtypes of nAChRs (i.e., Cholinergic Channel Activators, ChCAs) or inhibiting the function of other subtypes (Cholinergic Channel Inhibitors, ChCIs). An overview of the biology of nAChRs and the rationale for the use of ChCMs for the treatment of dementia related to neurodegenerative diseases are presented, followed by a discussion of lead compounds and compounds under consideration for clinical evaluation.