电化学发光法测定虎杖中白藜芦醇苷含量的研究

基于发现的白藜芦醇苷对 L uminol电化学发光强烈的抑制作用 ,建立了电化学发光法测定白藜芦醇苷含量的新方法。白藜芦醇苷浓度在 0 .0 5～ 12 .6 mg· L-1范围内与发光减少值分段呈良好的线性关系。检出限为0 .0 5 mg·L-1。对 0 .2 5 mg· L-1白藜芦醇苷平行测定 11次 ,其相对标准偏差为 2 .2 5 %。该法具有简便、快速、灵敏的特点 ,应用于中药虎杖中的白藜芦醇苷的测定 ,结果满意。     

HPLC法测定人血浆中曲唑酮的浓度

目的 :建立测定人血浆中曲唑酮 (TZD)浓度的RP HPLC法。方法 :以美国Dikma公司DiamonsilTMC18反相柱 (2 5 0mm×4 6mm ,5 μm)为色谱柱 ,流动相为甲醇 超纯水 (85∶15 ,V/V) ,流速为 0 8mL·min-1,检测波长 2 5 6nm ,以乙酸乙酯为提取剂。结果 :TZD高 (83 33mg·L-1)、中 (16 6 7mg·L-1)、低 (1 6 7mg·L-1) 3个浓度的平均回收率分别为 10 0 19% ,97 4 5 % ,95 5 1% ;日内、日间RSD均 <5 % (n =5 ) ;分析方法的最低检测浓度为 0 0 8mg·L-1。线性范围为 0 83～ 16 6 6 7mg·L-1,回归方程为Y =0 0 2 16X - 0 0 0 333,r=0 9999(n =10 )。结论 :该方法可用于临床TZD血药浓度监测和药动学研究     

高效液相色谱法同时检测人血清中3种抗癫痫药的浓度

目的　建立一种同时测定人血清中苯巴比妥 (PB)、苯妥英 (PT)和卡马西平 (CBZ) 3种抗癫痫药物的高效液相色谱(HPLC)定量方法。方法　采用C18色谱柱 ;流动相为甲醇 -水 (5 5∶4 5 ) ;内标物为巴比妥 (BB) ;检测波长为 2 2 0nm ;流速为 1 0ml·min-1;柱温为 30℃。结果　PB在 1 0～ 80mg·L-1范围内呈线性 (r =0 9999,n =5 ) ,PT在 1 0～ 5 0mg·L-1范围内呈线性 (r=0 9996 ,n =5 ) ,CBZ在 0 5～ 2 0mg·L-1范围内呈线性 (r =0 9995 ,n =5 ) ;其最低检测浓度分别为 0 2 5、0 2 5及 0 1mg·L-1;平均回收率分别为 95 75 %、96 5 4 %和 92 13% ;日内RSD(% )小于 6 2 9% ,日间RSD(% )小于 6 6 4 % (n =5 )。结论　本法简便、快速、灵敏 ,适用于癫痫病人血药浓度监测及药代动力学研究。     

国产与进口去氧氟尿苷胶囊在肿瘤病人体内药动学与生物等效性比较

目的 :以进口去氧氟尿苷胶囊为对照 ,考察国产去氧氟尿苷胶囊的药动学及 2种制剂的生物等效性。方法 :10名肿瘤病人随机双交叉口服 2种胶囊 80 0mg ,采用HPLC法测定药物的血药浓度。结果 :进口和国产去氧氟尿苷胶囊的药动学参数———Cmax分别为 (5 .1± 1.4 )mg·L- 1,(4.6± 1.2 )mg·L- 1;Tmax分别为 (1.0± 0 .4 )h ,(0 .8± 0 .4 )h ;AUC分别为 (6 .5± 1.7)mg·h·L- 1,(6 .0± 1.6 )mg·h·L- 1。国产去氧氟尿苷胶囊相对生物利用度为 (95± 12 ) %。结论 :2种制剂生物等效     

HPLC法测定甘草附子汤中甘草苷和香豆素的含量

目的建立HPLC法测定甘草附子汤中甘草苷和香豆素含量的方法。方法采用HypersilC18色谱柱 (2 0 0mm× 4 6mm ,5 μm) ,流动相为甲醇 乙腈 水 冰醋酸 (体积比 5∶1 5∶80∶1 ) ,流速0 8mL·min-1,检测波长 2 5 4nm。结果甘草苷在 2 0～ 3 0 0mg·L-1内成良好线性关系 ,平均回收率 95 9% ,RSD为 3 1 %。香豆素在 1 7～ 1 6 7mg·L-1内成良好线性关系 ,平均回收率 95 9% ,RSD为 2 0 %。结论本法可作为甘草附子汤质量控制的手段之一     

HPLC法测定白血病患者血浆中阿糖胞苷及其代谢物浓度

目的建立测定阿糖胞苷(Ara-C)及其代谢产物阿糖尿苷(Ara-U)血药浓度的方法,并用于5例急性髓细胞白血病(AML)患者血药浓度监测.方法采用反相离子对高效液相色谱法,色谱柱DiscoveryRC18柱(5μm,250mm×4.6mm);流动相乙腈-甲醇-0.01mo1·L-1磷酸盐缓冲液(pH4.0,含0.01 mo1·L-1戊烷磺酸钠)(4.51.594,v/v/v);流速1.0m1·min-1;检测波长280nm.结果以峰面积外标法定量,线性范围阿糖胞苷为0.25～25mg·L-1,阿糖尿苷为1～100mg·L-1.最低检测浓度阿糖胞苷为0.1mg·L-1,阿糖尿苷为0.2mg·L-1.日内、日间差阿糖胞苷小于9%和¨%,阿糖尿苷小于1%和3%.绝对回收率为99～105%.结论该方法简便,快速,灵敏度和准确度较高,能满足人体血药浓度监测及药代动力学研究的要求.     

一种简易的检测人血浆中喷昔洛韦浓度的HPLC法

目的 :建立一种简易的反相高效液相色谱法检测人血浆中喷昔洛韦浓度。方法 :用 10 %高氯酸沉淀血浆蛋白 ,三氯甲烷抽提血浆杂质成分 ,取上清液用HPLC分析。色谱柱为HypersilBDSC18,流动相为甲醇 -乙腈-磷酸盐缓冲液 (pH 7 0 ) (5∶0 1∶94 9) ,流速 :2 0mL·min-1。紫外检测波长为 2 5 4nm。结果 :喷昔洛韦与杂峰分离良好 ,最低检测限为 0 0 2 5mg·L-1。线性范围在 0 0 5～ 5mg·L-1。标准曲线回归方程C =0 0 0 12H- 0 0 386 (r =0 9999)。平均回收率为 93 7%～ 10 4 8%。结论 :本测定方法可满足泛昔洛韦和喷昔洛韦药代动力学和生物利用度研究的要求     

HPLC法同时测定徐长卿及老君须提取物中咖啡酸、橙皮苷、白薇苷A和胡萝卜苷含量

摘要：目的:建立HPLC法同时测定徐长卿及老君须提取物中咖啡酸、橙皮苷、白薇苷A和胡萝卜苷,并比较两种提取物中各成分的含量差异。方法:采用Agilent Zorbax C18色谱柱（250 mm×4.6 mm, 5μm）,以0.15%磷酸水（A）-乙腈（B）为流动相进行梯度洗脱,流速1 ml·min-1,柱温40℃,检测波长为260 nm和210 nm。结果:咖啡酸、橙皮苷、白薇苷A和胡萝卜苷分别在2.170 0～86.800 0 mg·L-1、5.412 5～216.500 0 mg·L-1、3.595 0～143.800 0 mg·L-1和4.090 0～163.600 0 mg·L-1范围内线性关系良好。通过研究发现,徐长卿提取物中咖啡酸、橙皮苷、白薇苷A和胡萝卜苷的含量分别为2.044 0,5.954 0,3.905 0,4.310 0 mg·g-1,而老君须提取物中仅可检测到白薇苷A和胡萝卜苷,含量分别为4.953,7.672 mg·g-1。结论:该方法简便、稳定,重复性好,可用于徐长卿及老君须提取物的质量评价。     

高效液相色谱法测定依托度酸及其在大鼠的药动学(英文)

目的 :建立测定依托度酸浓度的高效液相色谱法并研究该药在大鼠体内的药动学。方法 :血浆 2 0 0 μL加入 1 0 0mg·L-1 内标 (奥沙普秦) 50 μL ,酸化后用乙酸乙酯∶正己烷 (1∶1 9)提取。采用C1 8分析柱 ,以乙腈∶水∶三乙胺 (1 6∶84∶0 .0 0 2 )为流动相 ,流速为 1 .0mL·min-1 ;检测波长 2 80nm。大鼠按依托度酸 2 0mg·kg-1 剂量灌胃 ,给药前及给药后 5 ,1 0 ,2 0 ,30min和 1 ,3,6 ,1 2 ,2 4 ,48,72h采血 ,测定血浆药物浓度。绘制血药浓度 -时间曲线图并计算主要药动学参数。结果 :依托度酸与内标物的保留时间分别为 5 .2 8min和 6 .80min ;依托度酸浓度在1 .0～ 1 0 0 .0mg·L-1 范围内与依托度酸/内标物的峰面积比呈良好线性关系 ,回归方程为 :Y =0 .0 32 2 7C +0 .0 0 1 2 8,r =0 .9999,n =7。本法高、中、低浓度的绝对回收率为 73 .4 %～ 80 .5 % ,方法回收率在 97.3%～1 0 6.0 % ,日内RSD <4% ,日间RSD <8%。依托度酸的药动学参数为Tmax=0 .2 8h± 0 .1 3h ;Cmax=69mg·L-1 ± 5mg·L-1 ;T1 /2 =1 6 .9h± 2 .1h ;AUC =2 31 4mg·h·L-1 ±32 8mg·h·L-1 。结论 :本法快捷、灵敏、准确、重复性好 ,适用于依托度酸血药浓度测定及药动学研究。     

HPLC法测定人血清中多索茶碱浓度

目的 :建立测定人血清中多索茶碱浓度的RP HPLC法。方法 :以Techsphere ODS色谱柱为分析柱 ,流动相 :甲醇 水( 312∶4 88,V/V) ,流速为 0 8mL·min-1,检测波长为 2 73nm ,柱温为室温 ;血清样品经甲醇沉淀蛋白离心后进行色谱分析。结果 :本法在 0 75～ 2 0 0 0mg·L-1间线性关系良好 (r=0 9999) ,平均回收率为 99 2 1% ,日内及日间RSD均 <5 % ,最低检测血清浓度为 0 2 5mg·L-1。结论 :该方法快速、准确 ,适合多索茶碱临床药动学研究和血药浓度检测     

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.