HPLC法测定灯盏花素片含量

目的测定灯盏花素片的含量.方法采用高效液相色谱法.色谱柱为C18柱.(10μm,4.6mm×250mm);流动相为甲醇:水(80∶20);流速0.9ml*min-1,检测波长335nm;柱温:室温. 结果灯盏花素片在20μg～80μg*ml-1范围内,线性关系良好,平均回收率为100.2%,RSD为1.53%.结论该法可用于灯盏花素片中灯盏花乙素的含量测定.     

反相离子对色谱法分离加替沙星有关物质及其片剂含量测定

目的建立加替沙星有关物质的分离检测及其片剂的含量测定方法.方法采用反相离子对色谱(RPIC)法,色谱柱为ODS柱,流动相为0 .02mol*L-1磷酸二氢钾缓冲液(用磷酸调pH 4.5)-乙腈(82∶18)配制的0.003mo l*L-1四丁基溴化铵溶液,流速为1.0mL*min-1;检测波长为293nm,柱温为4 0℃.结果建立的色谱方法使有关物质与主药分离良好,加替沙星在4～40μg*mL-1范围内,浓度与峰面积线性关系良好,平均回收率100.2%,RSD=1.8%.结论本法简便、准确,可用于加替沙星有关物质的检查及片剂含量测定.     

马来酸氨氯地平片的高效液相色谱分析研究

目的建立马来酸氨氯地平片中马来酸氨氯地平及杂质的测定方法.方法采用高效液相色谱法,色谱柱Shim-Pack CLC-ODS(150mm×6.0mm)不锈钢柱,流动相甲醇-0.03mol*L-1磷酸二氢钾溶液(72∶28),检测波长237 nm,含量测定采用外标法,杂质检查采用面积归一化法.结果在优化的色谱条件下,氨氯地平、马来酸及杂质间均能完全分离,片剂辅料不干扰测定,马来酸氨氯地平线性范围1.0～120.0μg*mL-1,最低检测限0.2μg*mL-1,含量测定的回收率98.73%～100.9%,RSD<1.5%.结论该法专属性强,操作方便,结果准确,重现性好.     

RP-HPLC法测定加替沙星血药浓度

目的:建立高效液相色谱法测定血浆中加替沙星浓度.方法:血浆用二氯甲烷提取,色谱柱为ZorbaxC18(4.6mm×250mm),流动相为0.01mol*L-1磷酸二氢钾-甲醇-三乙胺(65∶34.8∶0.2),检测波长292nm,流速1.0ml*min-1,以司帕沙星为内标.结果:加替沙星浓度线性范围0.01～5μg*ml-1,最低检测浓度0.01μg*ml-1,绝对回收率为85.1%,相对回收率为100.6%.日内,日间RSD分别为3.0%和3.7%.结论:该方法适用于人体药物动力学研究.     

RP-HPLC法测定全血、血浆和红细胞中氯氮平及2种主要代谢物

目的建立一种测定全血、血浆和红细胞中氯氮平(CZP)、N-去甲基氯氮平(N-CZP)和氯氮平N-氧化物(CZP-NO)浓度的RP-HPLC法.方法标本用乙酸乙酯提取后再经0.1mol·L-1盐酸反提取,以利培酮为内标,流动相为甲醇-乙腈-水(16.0∶36.5∶47.5),色谱柱为Inertsil-ODS-3柱,柱温为40℃,检测波长为254nm,流速为0.9mL*min-1.结果全血、血浆和红细胞中CZP和N-CZP的最低检测浓度均为7μg*L-1;血浆中CZP-NO的最低检测浓度为13μg*L-1,全血和红细胞中为14μg*L-1.全血、血浆和红细胞中CZP和N-CZP的绝对回收率均为85%～95%,血浆中CZP-NO的绝对回收率>82%,全血和红细胞中CZP-NO的绝对回收率约为70%.日内和日间RSD均小于7%.结论本法操作简便,灵敏度高,重复性好,适合于临床检测.     

反相高效液相色谱法测定环孢素A血药浓度

目的采用RP-HPLC法测定环孢素A血药浓度.方法色谱柱为HypersilBDSC18柱(4.6mm×150mm,5μm),乙腈-水(62∶38)为流动相,柱温70℃,流速1.8ml*min-1,检测波长205nm.结果CsA血药浓度在50～1200ng*ml-1范围内,浓度与峰面积比有良好的线性关系,最低检测浓度为10ng*ml-1.平均回收率为(97.5±5.8)%(n=15).日内RSD≤6.8%,日间RSD≤9.6%.结论方法简单、快速、准确,可用于环孢素的临床药动学研究.     

高效液相色谱法测定人全血中瑞芬太尼浓度

目的:建立测定人血中瑞芬太尼的高效液相色谱-紫外检测方法,为临床监测血药浓度提供方法学.方法:采用液-液萃取法,用1-氯丁烷提取全血中的瑞芬太尼,选用GI97559(瑞芬太尼乙基类似物)为内标定量.色谱柱为Zorbax SB-CN(4.6 mm×250 mm,5 μm),流动相为乙腈-甲醇-磷酸二氢钠缓冲液(1∶2∶0.43),柱温30℃,流速1.5mL*min-1,紫外210 nm检测,按内标法定量.结果:标准曲线在3～200 μg*L-1范围内,浓度与峰面积比有良好的线性关系(r=0.9966).最低检测浓度为2μg*L-1.提取回收率77.34%～87.72%.方法回收率97.13%～100.99%,日内RSD小于5.3%,日间RSD小于6.3%.结论:本方法快速、准确、灵敏,可用于瑞芬太尼的临床药动学研究.     

高效液相色谱法同时测定滴鼻剂中三组分的含量

目的采用高效液相色谱(HPLC)法同时测定滴鼻剂中盐酸麻黄碱、盐酸苯海拉明、地塞米松磷酸钠的含量.方法采用C18色谱柱,流动相为甲醇-0.05 mol*L-1 KH2PO4-三乙胺(58∶42∶0.2),检测波长为221 nm.结果盐酸麻黄碱在1600～2400 mg*L-1浓度范围内线性关系良好(r=0.9994),回收率为99.8%,RSD为1.0%.盐酸苯海拉明80～120 mg*L-1浓度范围内线性关系良好(r=0.9996),回收率为101.0%,RSD为0.9%.地塞米松磷酸钠160～240 mg*L-1浓度范围内线性关系良好(r=0.9991),回收率为99.6%,RSD为0.8%.结论该方法可同时测定滴鼻剂中盐酸麻黄碱、盐酸苯海拉明、地塞米松磷酸钠.     

高效液相色谱法测定头孢他啶注射剂的含量

目的建立用高效液相色谱法测定头孢他啶注射剂含量的方法.方法以甲硝唑为内标,所用色谱柱为ODS柱,流动相为磷酸盐缓冲液(含0.08%NaH2PO4,pH=4.7)-甲醇＝9∶1,流速1.5ml*min-1,检测波长为254nm.结果在5.0～50.0μg*ml-1的浓度范围内具有良好的线性关系,r＝0.9999.平均回收率为100.6%,RSD＝0.79%.与中国药典2000年版方法相比,差异无显著性(P>0.05).结论采用内标法测定简便,快速,灵敏,准确.     

HPLC法测定吲哚美辛片剂的含量

建立吲哚美辛片剂HPLC含量测定方法.用Kromasil TM C18色谱柱(4.6mm×250mm,5μm),以甲醇-0.01mol*L-1磷酸二氢钾溶液(85∶15)(用磷酸调pH至2.6)为流动相,流速为1.0ml*min-1,检测波长为320nm.吲哚美辛在1.899～37.980μg*ml-1范围内呈良好的线性关系,r=0.9998,平均回收率为100.07%,RSD=0.39%(n=5).本法适用于吲哚美辛片剂的含量测定.     

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.

---

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.