UPLC法同时测定消积化虫散中3种成分的含量

摘 要 目的：建立UPLC同时测定消积化虫散中橙皮苷、和厚朴酚、厚朴酚3种成分含量的分析方法。方法: 采用Thermo Accucore C18（150 mm×4.6 mm, 2.6 μm）,以甲醇 0.5%冰醋酸水溶液为流动相进行梯度洗脱,流速：0.7 ml·min^-1 ,柱温：30℃,检测波长：283 nm,进样量：2 μl。结果: 橙皮苷、和厚朴酚、厚朴酚分别在4.707~28.242 mg·ml^-1 (r=0.999 4)、5.085~30.510 mg·ml^-1 (r=0.999 7)、10.651~63.908 mg·ml^-1 (r=0.999 5)浓度范围内线性关系良好,平均加样回收率分别为101.2%,104.8%,99.4%,RSD分别为1.11%,1.68%,1.49%（n=6）。结论: 本试验为消积化虫散的质量评价提供了简单、有效的方法。     

HPLC法测定黄连上清片中4种成分的含量

摘 要 目的： 提高黄连上清片质量标准,建立同时测定绿原酸、栀子苷、黄芩苷、盐酸小檗碱4种成分含量的方法。方法: 采用高效液相色谱法,色谱柱为DiamonsilTM C₁₈(250 mm×4.6 mm,5 μm),流动相为二元梯度系统,其中溶剂A为乙腈,溶剂B为0.3%磷酸水溶液,流速为1.0 ml·min^-1,检测波长为238 nm,柱温30℃,进样量为10 μl。结果: 绿原酸、栀子苷、黄芩苷、盐酸小檗碱的线性范围分别为8.11～81.10 μg·ml^-1(r=0.999 7)、13.08～130.80 μg·ml^-1(r=0.999 7)、10.76～107.60 μg·ml^-1(r=0.999 8)、7.92～79.20 μg·ml^-1(r=0.999 8)范围内呈良好的线性关系,平均加样回收率分别为99.19%(RSD=0.9%)、98.44%(RSD=1.1%)、99.12%(RSD=1.0%)、99.18%(RSD=1.1%)(n=9)。结论:该方法简便、准确、重复性好,可用于黄连上清片的质量控制。     

HPLC法同时测定神农茶颗粒中的夏佛塔苷、异夏佛塔苷、去氧地胆草内酯和4,5-二咖啡酰奎宁酸

摘 要 目的： 建立同时测定神农茶颗粒中夏佛塔苷、异夏佛塔苷、去氧地胆草内酯、4,5-二咖啡酰奎宁酸4个成分的高效液相色谱测定方法。 方法: 采用Hypersil C₁₈色谱柱（200 mm×4.6 mm,5 μm）;以乙腈 0.025 mol·L^-1磷酸溶液为流动相进行梯度洗脱,体积流量：1.3 ml·min^-1,检测波长：270 nm（夏佛塔苷和异夏佛塔苷）、208 nm（去氧地胆草内酯）、327 nm（4,5-二咖啡酰奎宁酸）,柱温为室温。结果:夏佛塔苷、异夏佛塔苷、去氧地胆草内酯和4,5-二咖啡酰奎宁酸分别在5.850～117.000,4.650～93.000,4.160～83.200,5.470～109.400 μg·ml^-1范围内线性良好,r值均大于0.999,平均加样回收率分别为97.70％、96.87％、97.53％、99.29％,RSD分别为1.40％、1.13%、1.69%、1.01％(n=6)。 结论: 该方法简便,结果准确,可用于神农茶颗粒的含量测定。     

HPLC法测定追风舒筋活血片中马钱子碱、士的宁的含量

摘 要 目的： 建立追风舒筋活血片中马钱子碱、士的宁的含量测定方法。方法: 应用高效液相色谱法测定,色谱柱为Agilent SB C₁₈柱(250 mm×4.6 mm,5 μm),以乙腈 0.01 mol·L^-1庚烷磺酸钠与0.02 mol·L^-1磷酸二氢钾等量混合溶液（用10%磷酸调节pH至2.8）（21∶79）为流动相,检测波长为260 nm,流速为1.0 ml·min^-1,柱温为35℃,进样量为10 μl。结果: 马钱子碱和士的宁的线性范围分别为0. 011 0~0.219 6 mg·ml^-1 (r=0.999 4)、0.010 1~0.202 8 mg·ml^-1 (r=0.999 7);平均加样回收率分别为98.24%(RSD=1.54%)、97.92%(RSD=1.49%)(n=6) 。结论:该方法简便易行、准确、重复性好,可用于追风舒筋活血片的质量控制。     

HPLC法测定吲哚美辛呋喃唑酮栓中两组分的含量

摘 要 目的：建立同时测定吲哚美辛呋喃唑酮栓中两组分含量的HPLC法。方法: 采用XTerra RP18色谱柱(250 mm×4.6 mm,5 μm),以甲醇为流动相A,0.01 mol·K^-1磷酸二氢钾溶液 三乙胺(100〖KG*9〗∶〖KG-*2〗0.02)为流动相B,梯度洗脱,流速1.0 ml·min^-1,柱温30 ℃,检测波长263 nm,进样量10 μl。结果: 吲哚美辛呋喃唑酮栓中呋喃唑酮和吲哚美辛的分离度符合要求;线性范围分别为5.12~81.87 μg·ml^-1 (r=1.000 0)和3.78~60.45 μg·ml^-1 (r=1.000 0);平均回收率分别为99.6% (RSD=1.5%,n=6)和100.3% (RSD=1.6%,n=6);定量限分别为0.02 μg·ml^-1和0.05 μg·ml^-1。结论:该法经方法学验证,适用于吲哚美辛呋喃唑酮栓的质量评价。     

HPLC法同时测定蒲药灌肠液中3个有效成分的含量

摘 要 目的： 建立蒲药灌肠液中香蒲新苷、异鼠李素-3-O-新橙皮苷和延胡索乙素的HPLC含量测定方法。方法: 采用ZORBAX SB-C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以乙腈-0.1%磷酸（三乙胺调节pH至6.0）为流动相,梯度洗脱程序,流速:1.0 ml·min^-1,检测波长为254 nm（0～14 min）和281 nm（14～25 min）,柱温:30 ℃。结果: 香蒲新苷、异鼠李素-3-O-新橙皮苷和延胡索乙素的线性范围分别为19.840～198.400 μg·ml^-1（r=0.999 6）、20.520～205.200 μg·ml^-1（r=0.999 8）和10.040～100.400 μg·ml^-1（r=0.999 7）,回收率分别为98.8%、98.6%和98.9%,RSD分别为1.4%、1.6%和1.3%（n=6）。结论: 该方法灵敏度高,专属性强,可用于蒲药灌肠液的质量控制。     

HPLC波长切换法测定氨咖黄敏胶囊4个成分的含量

摘 要 目的： 建立HPLC波长切换法同时测定氨咖黄敏胶囊中4个成分的含量。方法: 采用Agilent ZORBAX SB C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以乙腈（A）-甲醇（B）-磷酸二氢铵溶液（取0.1 mol·L^-1磷酸二氢铵溶液1 000 ml ,加磷酸1 ml,混匀）（C）为流动相,梯度洗脱,流速1.0 ml·min^-1,柱温 35℃,变换波长时间为（0～9 min ：225 nm;9～38 min ：450 nm）。结果: 采用HPLC波长切换法测定氨咖黄敏胶囊4个成分的含量,线性范围分别为：对乙酰氨基酚24.680～394.900 μg·ml^-1（r=0.999 9）,马来酸氯苯那敏0.201～3.214 μg·ml^-1（r=0.999 9）,咖啡因1.129～18.070 μg·ml^-1（r=0.999 9）,胆红素0.010～0.165 μg·ml^-1（r=0.999 8）;平均回收率分别为：99.25% (RSD=0.46%), 99.29% (RSD=0.32%),99.49% (RSD=0.48%)及99.75% (RSD=0.55%)（n=6）。结论:该法简单,灵敏,准确,重复性好,可用于氨咖黄敏胶囊的含量测定。     

离子色谱法测定枸橼酸氢钾钠颗粒中多种成分的含量

摘 要 目的：建立离子色谱法测定枸橼酸氢钾钠颗粒中钠、钾和枸橼酸含量的方法。方法: 钾和钠的色谱条件：采用Dionex IonPac CS12A色谱柱（250 mm×4.6 mm,5 μm）,流动相为0.02 mol·L^-1甲烷磺酸溶液,流速为1.0 ml·min^-1,抑制器为CSRS 300,抑制电流为59 mA,采用抑制型电导检测器,进样量为25 μl。枸橼酸的色谱条件：采用Dionex HPICE AS1离子排斥色谱柱（250 mm×9.0 mm,7.5 μm）,流动相为0.015 mol·L^-1硫酸溶液,流速为0.6 ml·min^-1,检测波长为220 nm,进样量为10 μl。结果: 钠的线性范围为0.82～82.49 μg·ml^-1（r=0.999 9）,平均回收率为98.9%,RSD为0.55% （n=9）;钾的线性范围为1.38～137.89 μg·ml^-1（r=1.000 0）,平均回收率为100.5%,RSD为0.53%（n=9）;枸橼酸的线性范围为0.021～10.600 mg·ml^-1（r=1.000 0）,平均回收率为99.1%,RSD为0.54%（n=9）。结论:本方法简便、快速、准确,可用于枸橼酸氢钾钠颗粒的质量控制。     

HPLC法同时测定蛇胆追风丸中阿魏酸、蛇床子素的含量

摘 要 目的： 采用HPLC法同时测定蛇胆追风丸中阿魏酸、蛇床子素的含量。方法: 采用Phenomenex Synergi C₁₈(250 mm×4.6 mm,4 μm)色谱柱,流动相为甲醇 0.1%磷酸,梯度洗脱,检测波长为322 nm,流速为1.0 ml·min^-1。结果: 阿魏酸、蛇床子素线性范围分别为1.244～14.928 μg·ml^-1(r＝0.999 9)、5.004～25.020 μg·ml^-1(r＝0.999 8),平均加样回收率分别为98.3%(RSD=1.4%,n=6)、98.2%(RSD=1.6%,n=6)。结论: 该方法操作简便,结果准确可靠,可作为蛇胆追风丸中阿魏酸、蛇床子素的含量测定方法。     

HPLC法测定金沙牛化石片中夏佛塔苷含量

摘 要 目的：建立高效液相色谱法测定金沙牛化石片中夏佛塔苷的含量。方法: 采用Agilent ZORBAX SB C₁₈色谱柱（150 mm×4.6 mm, 5μm）,以0.2%磷酸 乙腈为流动相进行梯度洗脱,流速为1.0 ml·min^-1,检测波长为272nm,柱温为25℃。 结果: 夏佛塔苷在4.58~183.15 μg·mL^-1浓度范围内与峰面积呈良好线性关系（r=1.000 0）,平均加样回收率为99.65%（n=6）,RSD为1.09%。结论:该方法简单、准确,具有良好的重复性和稳定性,可用于金沙牛化石片中夏佛塔苷的含量测定。     

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.