丙泊酚中/长链脂肪乳注射液中溶血磷脂酰胆碱和溶血磷脂酰乙醇胺的含量测定

目的建立HPLC法测定丙泊酚中/长链脂肪乳注射液中溶血磷脂酰胆碱(LPC)和溶血磷脂酰乙醇胺(LPE)的含量。方法采用HPLC法,色谱柱:Lichrospher 100 DIOL(250 mm×4 mm,5μm);流动相:乙腈-水-冰醋酸-三乙胺(85∶15∶0.45∶0.05)为流动相A,正己烷-异丙醇(18∶30)溶液为流动相B;梯度洗脱;柱温:35℃。结果溶血磷脂酰胆碱和溶血磷脂酰乙醇胺的线性范围分别为0.03~0.25(r1=0.9997)和0.01~0.10(r2=0.9962)mg·mL^-1,定量限分别为0.72和0.31μg。结论该方法准确、可行,精密度高,可用于溶血磷脂酰胆碱和溶血磷脂酰乙醇胺的含量测定。     

高效液相色谱法测定多烯磷脂酰胆碱软胶囊中磷脂酰胆碱和溶血磷脂酰胆碱的含量

目的建立HPLC法测定多烯磷脂酰胆碱软胶囊中磷脂酰胆碱和溶血磷脂酰胆碱的含量以及有关物质方法。方法采用蒸发光散射检测器SEDEX55,MERCK的Li Chrospher 100 Diol-5色谱柱(125mm×4.0 mm,5μm);流动相A为正己烷-异丙醇-冰醋酸-三乙胺(814∶170∶15∶0.8),流动相B为异丙醇-超纯水-冰醋酸-三乙胺(844∶140∶15∶0.8),梯度洗脱。结果磷脂酰胆碱在0.912~2.736mg·mL~(-1),溶血磷脂酰胆碱在0.072~0.216 mg·mL~(-1)内与峰面积线性关系良好(R~2均为0.999)。磷脂酰胆碱的平均回收率为101.2%,RSD为1.3%;溶血磷脂酰胆碱的平均回收率为100.5%,RSD为1.9%。溶血磷脂酰胆碱的检测限为0.57μg。结论本检测方法专属性强,结果可靠,专属性强,重复性良好,可用于多烯磷脂酰胆碱软胶囊的质量评价。     

HPLC测定多烯磷脂酰胆碱胶囊中的溶血磷脂酰胆碱

目的 采用HPLC-ELSD测定多烯磷脂酰胆碱胶囊中溶血磷脂酰胆碱的含量.方法 色谱柱为硅胶(250 mm×4.6mm,5 μm),流动相A为正己烷-异丙醇(3:4),流动相B为正己烷-异丙醇-水(3:4:0.75),梯度洗脱,流速为1.5 mL·min~(-1),空气流速为3.0 L·min~(-1),蒸发管温度为100 ℃.结果 溶血磷脂酰胆碱0.1～1.5 mg·mL~(-1)与峰面积呈良好的线性关系(r=0.9997),平均回收率为99.90%.结论 所用方法简便、专属性好,可用于多烯磷脂酰胆碱胶囊中溶血磷脂酰胆碱的含量检测.     

HPLC-ELSD多烯磷脂酰胆碱质量标准研究

目的 建立多烯磷脂酰胆碱胶囊中多烯磷脂酰胆碱含量及溶血磷脂酰胆碱的限量检查.方法 丙二醇键合硅胶色谱柱(5μM,4.6 ×250 mm,Hanbon),柱温:55℃,流动相:A为正己烷-异丙醇-冰醋酸-三乙胺(814∶170∶15∶1.4),B为异丙醇-水-冰醋酸-三乙胺(844∶140∶15∶1.4),梯度洗脱,流速:1ml·min-1,蒸发光散射检测器物化温度50℃,蒸发温度90℃,载气流速2.0ml·min-1.结果 多烯磷脂酰胆碱在0.1～1 mg·mL-1范围内呈良好线性,r=0.9999;平均回收率为100.1%,RSD为1.7%;中间精密度RSD为1.4%;三批样品中多烯磷脂酰胆碱的标示量%分别为100.9%,99.84%,100.2%,溶血磷脂酰胆碱的含量占多烯磷脂酰胆碱表示量的3.9%,4.4%,3.9%.本样品中磷脂酰乙醇胺未检出.结论 所建立的方法可准确的测定胶囊中多烯磷脂酰胆碱的含量及溶血磷脂酰胆碱的限量检查,可用于该制剂的质量控制.     

HPLC—ELSD法测定复合磷脂固醇脂质中磷脂酰胆碱的含量

目的:采用 HPLC-ELSD 法测定复合磷脂固醇脂质中磷脂酰胆碱(PC)的含量。方法:采用 Waters Nova-pak(?) silica60(?)径向柱(100 mm×8 mm,4 μm),流动相:己烷-异丙醇(3:4)为流动相 A,己烷-异丙醇-水(3:4:0.75)为流动相 B,梯度洗脱,流速1.5 mL·min~(-1);蒸发光散射检测,ELSD 漂移管温度:40℃,雾化气:氮气,载气压力:340 kPa。结果:在选定的色谱条件下,棕榈酸甘油三酯、磷脂酰乙醇胺、溶血磷脂酰乙醇胺、磷脂酰胆碱、鞘磷脂、溶血磷脂酰胆碱各成分之间可达到很好分离。磷脂酰胆碱进样量在21.2～127.2 μg范围内与峰面积的线性关系良好(r=0.9969),最低检测限为424 ng(S/N=3),3个浓度水平下磷脂酰胆碱的平均同收率(n=9)为100.6%。结论:方法灵敏,快速,准确,重复性好,可用于产品的质量控制。     

HPLC-ELSD测定大豆磷脂中溶血磷脂酰胆碱的含量

目的:采用HPLC-ELSD法测定大豆磷脂中溶血磷脂酰胆碱(LPC)的含量。方法:采用NH2柱(150 mm×4.6 mm,5μm),柱温为30℃,流速为0.8 mL.min-1,进样量为10μL。流动相:甲醇-氯仿(97∶3)为流动相A,草酸-乙醇(16∶84)为流动相B,A∶B=7∶3;蒸发光散射检测,ELSD漂移管温度:80℃,雾化气:空气,气体流量:2.0 L.min-1。结果:在选定的色谱条件下,大豆磷脂和溶血磷脂酰胆碱之间可达到很好分离。溶血磷脂酰胆碱进样量在0.2~3.2 mg范围内与峰面积的线性关系良好(r=0.999 3),最低检测限为80 ng(S/N=3),3个浓度水平下溶血磷脂酰胆碱的平均回收率(n=9)为100.1%。结论:该方法灵敏、快速、准确,可用于产品的质量控制。     

HPLC-ELSD测定尼莫地平脂肪乳注射液中溶血磷脂酰胆碱的含量

目的：建立HPLC-ELSD测定尼莫地平脂肪乳注射液中溶血磷脂酰胆碱（LPC）的含量.方法：采用Kromasil 100-5SIL（250 mm×215;4.6 mm,5 μm）色谱柱,以甲醇-冰醋酸（500：10,三乙胺调节pH至6.0） 为流动相,流速为1.0 ml·min^-1,柱温为30℃,使用蒸发光散射检测器（雾化气：氮气,漂移管温度：60℃）.结果：样品中磷脂酰胆碱（PC）及LPC与相邻杂质峰分离效果良好;LPC定量限为218.2 ng,检测限为65.46 ng;平均回收率为100.9%,RSD为3.3%（n=9）.结论：本法简便、专属性强、准确可靠,可用于尼莫地平脂肪乳注射液中溶血磷脂酰胆碱的含量测定.     

HPLC法测定卵磷脂中6个成分的含量

目的:采用HPLC法测定卵磷脂中6个成分的含量。方法:采用LiChrosphere 100 DIOL色谱柱(250 mm×4mm,5μm),以正庚烷∶异丙醇(65∶114)为流动相A,正庚烷∶异丙醇∶水(31∶62∶12)为流动相B,梯度洗脱,流速0.8mL/min,用蒸发光散射检测器进行检测。结果:磷脂酰胆碱和磷脂酰乙醇胺的线性范围分别为1.69~33.76μg(r=0.997 9),0.33~6.57μg(r=0.999 6),棕榈酸甘油酯、胆固醇、鞘磷脂和溶血性磷脂酰胆碱的最低检测限分别为0.3、3、10和20 ng。结论:本方法操作简便、准确,可用于卵磷脂中各个成分的测定。     

HPLC法测定多烯磷脂酰胆碱注射液中多烯磷脂酰胆碱和苯甲醇的含量

分别建立了HPLC法测定多烯磷脂酰胆碱注射液中多烯磷脂酰胆碱和防腐剂苯甲醇的含量.多烯磷脂酰胆碱的测定采用正相硅胶柱,流动相为异丙醇-正己烷-水(66:14:20),检测波长为205 nm,线性范围为0.585 3～1.365 8 mg/ml,平均回收率为100.1%.苯甲醇的测定采用反相辛基硅烷键合硅胶柱,流动相为乙腈-磷酸盐缓冲液(己烷磺酸钠0.942%,pH2.5)(3:7),检测波长为256 nm,线性范围为0.597 6～1.394 4 mg/ml,平均回收率为99.95%.     

不同生产厂家的中/长链脂肪乳注射液质量评价

目的了解不同生产厂家中/长链脂肪乳注射液的质量差异。方法从医药流通市场购买不同生产厂家的中/长链脂肪乳注射液各3个批次,对其pH值、平均粒径、粒径分布、游离脂肪酸、过氧化值、甲氧基苯胺值、溶血磷脂酰胆碱与溶血磷脂酰乙醇胺、甘油、渗透压摩尔浓度、含量等进行测定与对比。结果共分析6个不同生厂家的中/长链脂肪乳注射液,受试批次pH值为7.4~8.3;平均粒径为0.181~0.298μm;>5μm百分比为0.93×10^-3%~34.5×10^-3%;游离脂肪酸均为0.01 mmol/g;过氧化值均未检出;甲氧基苯胺值为0.8~1.7;溶血磷脂酰胆碱为0.5~0.9 mg/mL;溶血磷脂酰乙醇胺为0.1~0.2 mg/mL;甘油为2.46~2.59mg/mL;渗透压摩尔浓度为372~404 mOsmol/kg;大豆油为93.8%~103.4%;中链甘油三酸酯为98.5%~102.1%;α-生育酚为0.000%~0.018%。结论6个不同生产厂家的中/长链脂肪乳注射液3个批次均符合中/长链脂肪乳注射液国家标准公示稿要求。     

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.     

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.