槐角丸中4种有效成分的高效毛细管电泳法测定

建立了高效毛细管电泳法分离测定槐角丸中的4种有效成分——染料木素、芸香苷、黄芩苷、没食子酸。采用未涂层石英毛细管柱，以15mmol／L硼砂缓冲液（pH9．0）-5mmol／L磷酸二氢钠溶液为运行缓冲液，检测波长214nm。以槲皮素为内标，槐角丸中4种有效成分在12min内分离良好，分别在4．96～29．76、12．80～76．80、17．20～103.20和10.44～62．64μg/ml浓度范围内线性关系良好。     

短毛细管区带电泳快速测定增效联磺片中三组分含量

目的:在短毛细管上应用毛细管区带电泳法快速测定增效联磺片中磺胺甲嗯唑(SMZ)、磺胺嘧啶(SD)及甲氧苄氨嘧啶(TMP)三组分的含量。方法:采用未涂层弹性石英毛细管(35cm×50 μm,有效长度20 cm),以咖啡因为内标(IS),检测波长214 nm(0.01 AUFS),电压10 kV,重力进样(10 cm×5 s),温度15℃,运行缓冲液为20 mmol·L-1硼砂溶液(磷酸调pH6.0)。每次电泳运行前用0.1 mol·L-1氢氧化钠溶液、水及缓冲溶液各冲洗毛细管3 min。结果:SMZ、SD、TMP的线性范围分别为0.0398-0.199,0.0399-0.200,0.0160-0.0800 mg·mL-1。平均回收率(n=9)分别为99.4％,99.0％,99.8％;RSD均小于1.5％。结论:该法简便快捷,准确可靠,灵敏度高。     

紫外分光光度法测定染料木素胶囊含量及溶出度

目的:建立了测定染料木素胶囊含量和溶出度的方法。方法:利用染料木素与氢氧化钠能产生颜色反应,在271nm波长处有最大吸收的特点,用紫外分光光度法测定染料木素胶囊中染料木素的含量,并用中国药典溶出度测定第一法,以0.01mol·L-1氢氧化钠溶液为溶出介质,转速100 r·min～1,用建立的紫外分光光度法进行检测。结果:染料木素浓度在2.04—6.12μg·mL-1范围内,与吸收度呈良好线性关系(r=0.9999),平均回收率为99.76％,RSD为0.92％(n=6);胶囊在30 min时的溶出量均不少于标示量的95％。结论:此法简单、准确,可作为染料木素胶囊质量控制标准之一。     

高效毛细管电泳分离和测定注射用盐酸吉西他滨中有关物质

目的:建立高效毛细管电泳法分离盐酸吉西他滨差向异构体以及胞嘧啶,测定注射用盐酸吉西他滨的杂质盐酸吉西他滨α异构体及胞嘧啶含量。方法:采用熔融石英毛细管:总长60 cm,检测端38cm,内径50 μm;以pH 3.5的0.05 mol·L-1磷酸盐缓冲液为运行缓冲液,运行电压为21 kV,柱温:25℃,检测波长为275 nm,真空进样5 s。结果:胞嘧啶及盐酸吉西他滨α异构体和β异构体分离完全,线性范围分别为7.0—140μg·mL-1(r=0.9994),5.0-100μg·mL-1(r=0.9996),5.8—117μg·mL-1(r=0.9996),n=5;精密度(RSD)分别为1.7％,1.9％,2.1％(n=5),最低检测浓度分别为0.5,1.0,1.2μg·mL～1。结论:方法快速、简便且准确,可用于盐酸吉西他滨的杂质盐酸吉西他滨α异构体及胞嘧啶含量的测定。     

胶束动电毛细管电泳色谱法分离测定卫非宁片中的异烟肼和利福平

目的:应用胶束动电毛细管电泳(MECC)技术分离测定卫非宁片中的异烟肼和利福平。方法:以0.02mol·L~(-1)磷酸盐缓冲液(pH 10.0)为运行液,分离电压18kV(运行电流150～180μA),检测波长214nm,柱温25℃,重力法进样10s,选择苯巴比妥为内标物。结果:卫非宁片中的2种成分在15min内达到完全基线分离。在0.1～0.55mg·mL~(-1)浓度范围内,浓度与峰面积呈良好的线性关系。2种成分的加样回收率分别为106.30％和103.24％,RSD均小于4％。结论:胶束动电毛细管电泳色谱法测定卫非宁片中的两种成分准确可靠,且简便易行。     

毛细管电泳法测定冬虫夏草中核苷类的含量

目的 :探讨毛细管电泳法测定天然和人工冬虫夏草中腺苷、鸟苷和尿苷等核苷含量的可行性。方法 :采用BeckmanP ACESystem 5 0 10高效毛细管电泳仪 ,Beckman无涂层毛细管 (5 7cm× 75 μm ,有效长度 5 0cm) ,自动压力 (5 86kPa)进样6s ,检测波长 2 5 4nm ,电压 2 0kV ,温度 2 0℃ ,运行缓冲液为 0 2mol·L- 1 硼酸 (用 5mol·L- 1 氢氧化钠溶液调pH 8 5 )。进样前 ,毛细管分别以 1mol·L- 1 氢氧化钠溶液和运行缓冲液冲洗 5min。结果 :该法平均回收率腺苷为 97 0 % ,鸟苷为98 4% ,尿苷为 97 1% ;RSD分别为 0 72 % ,0 6 7% ,0 6 2 % (n =6 )。结论 :该法快速简便 ,灵敏度高 ,重现性好。     

高效毛细管电泳法测定地塞米松磷酸钠脂质体中地塞米松磷酸钠的含量

目的:建立高效毛细管电泳法测定地塞米松磷酸钠脂质体中药物含量。方法:毛细管(60 cm×75μm,有效长度53cm);运行缓冲液100 mmol·L-1硼砂(0.1 mol·L-1盐酸调pH 9.2),高压进样5 s,分离电压20 kV,温度为20℃,头孢拉定为内标,检测波长为240 nm。结果:地塞米松磷酸钠在0.78-50 μg·mL-1浓度范围内线性关系良好(r=0.9998),地塞米松磷酸钠的平均回收率为98.5％。结论:本方法准确、简单、快捷,适用于地塞米松磷酸钠脂质体的质量控制。     

毛细管电泳法测定富马酸托特罗定S型异构体

目的　测定R型富马酸托特罗定中的S型异构体。方法　采用 6 8cmⅹ 5 0 μm的毛细管 ,以含 0 0 1mol·L-1羟丙基环糊精的三羟甲基氨基甲烷溶液 (磷酸调pH 2 5 )为缓冲液 ,运行电压为 30kV ,毛细管温度 15℃ ,检测波长 2 0 4nm ,压力进样 10 0mbar·s-1。结果　最低检出浓度 0 0 12mol·L-1,平均加样回收率为 10 1 2 9% ,RSD =1 5 % (n =6 )。结论　毛细管电泳法用于测定R型富马酸托特罗定中的S型异构体 ,方法简便快捷 ,灵敏度高 ,重复性好     

复方石韦片中生物碱的分离测定

目的:建立了复方石韦片中槐果碱和苦参碱的分离测定方法。方法:采用高效毛细管电泳法进行测定。运行电压27kV;运行缓冲液为0.2 mol·L~(-1) Tris-40 mmol·L~(-1)磷酸二氢钠-5％异丙醇,磷酸调pH 5.75;进样方式:真空进样;进样时间:5s;检测波长:205nm。结果:槐果碱和苦参碱的线性范围分别为0.5～5.76μg·mL~(-1)和0.66～13.2μg·mL~(-1),相关系数分别为0.9991和0.999 3,平均回收率分别为99.5％和99.3%,RSD分别小于4％和2％(n=3)。结论;本法简便、快速、重现性好。     

毛细管电泳法同时测定元胡止痛片中欧前胡素和异欧前胡素的含量

目的:建立以毛细管电泳法同时测定元胡止痛片中欧前胡素和异欧前胡素含量的方法。方法:以盐酸小檗碱为内标,采用未涂层弹性融硅石英毛细管柱(55cm×75μmID,有效长度47cm),以20mmol·L-1磷酸二氢钠+100mmol·L-1十二烷基磺酸钠+80%甲酰胺溶液(pH7.12)为运行缓冲液,分离电压为15kV,重力进样5s(高度15cm),检测波长为254nm。结果:欧前胡素、异欧前胡素检测浓度分别在8.0～40.0μg·mL-(1r=0.9987)、4.0～20.0μg·mL-(1r=0.9990)范围内与各自峰面积积分值呈良好线性关系;二者平均回收率分别为101.3%和100.2%,RSD分别为3.24%和1.44%(n=6)。结论:本法简便、快速、准确,可用于元胡止痛片的质量控制。     

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.     

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.     

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.     

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.