固相萃取-高效液相色谱法测定人体血浆中阿奇霉素的浓度

目的:建立人体血浆中阿奇霉素 HPLC 测定法。方法:血样采用固相萃取方法,即2.0 mL 血浆过柱抽干后,用1.0 mL双蒸水连续淋洗2次,淋洗液弃去,再用1.0 mL 甲醇洗脱回收,回收液于60℃水浴挥干,最后用100 μL流动相溶解残渣,取30 μL进样。流动相为0.03 mol·L~(-1)磷酸二氢钾缓冲液(pH=4.5)-甲醇-乙腈(72:18:10);流速为1.0 mL·min~(-1);色谱柱为 C_(18)柱(4.6 mm×250 mm,5μm);柱温为室温;检测波长为210 nm。结果:阿奇霉素在0.01～1.44 mg·L~(-1)范围内线性关系良好(r=0.9994),最低检测浓度为0.008 mg·L~(-1),方法回收率在98.6%～104.4%,日内、日间 RSD 均小于5.6%。结论:该方法快速、灵敏、准确,可用于人体血浆中阿奇霉素浓度的测定。     

HPLC法测定阿奇霉素片的含量

目的:建立HPLC法测定阿奇霉素片的含量.方法:采用Shodex Asahipak ODP-50(4.6 mm×250mm,5μm)C18柱,流动相为0.04 moL·L-1磷酸氢二钾溶液(称取6.97 g磷酸氢二钾,加水750 mL使溶解,用1moL·L-1的氢氧化钾溶液调节pH值至11.0±0.1再加水稀释至1 000 mE)-乙腈(40:60),流速为1.0 mE·min-1,检测波长为215 mn;柱温40℃;结果:阿奇霉素的线性范围为2.187～8.399 g·L-1,平均回收率为99.9%(RSD 0.15%).结论:本方法简便、迅速、灵敏度高、重现性好,可用于测定阿奇霉素片的含量.     

HPLC法测定注射用阿奇霉素磷酸二氢钠的含量及有关物质

目的建立一种高效液相色谱方法来测定注射用阿奇霉素磷酸二氢钠含量及有关物质。方法以Shiseido C18(4.6 mm×250 mm,5μm)色谱柱为分析柱,以磷酸盐缓冲液(0.05 mol·L-1磷酸氢二钾溶液,用20%磷酸溶液调节pH值至8.2)-乙腈(40∶60)为流动相,柱温30℃,检测波长为210 nm,流速为1.0 mL·mim-1。结果阿奇霉素在10⁵ 000μg·mL-1范围内浓度与峰面积呈良好线性关系,r=1.000 0,平均回收率为100.6%,RSD为0.99%(n=9)。结论本方法可快速、准确的测定注射用阿奇霉素磷酸二氢钠含量及有关物质的测定。     

高效液相色谱法测定阿奇霉素胶囊含量

目的建立高效液相色谱法测定阿奇霉素胶囊含量。方法色谱柱为Hypersil ODS2(4.6×250 mm);流动相为0.067 mol.L-1磷酸二氢钾溶液(用磷酸调pH为3.5)-乙腈(70∶30);流速为1.0 ml.min-1;柱温:50℃;检测波长:210 nm。结果阿奇霉素在进样量2.5~50μg的范围内与峰面积呈良好线性关系(r=0.9999),平均回收率为100.38%,RSD为0.91%。结论本法简便快捷,结果准确,重现性好,可用于阿奇霉素胶囊的含量测定。     

高效液相色谱法测定阿奇霉素的含量

目的:用高效液相色谱法测定阿奇霉素的含量.方法:以日本岛津CLC-CN柱为固定相,0.1 mol·L-1磷酸二氢钠-甲醇-乙腈(85∶7∶8)为流动相,在pH 3.0～3.5,流速:1 mL·min-1,柱温:40 ℃,紫外检测波长210 nm,灵敏度为0.08 AUFS的条件下分离测定阿奇霉素,并对方法进行了认证.结果:阿奇霉素与其杂质能完全分离,在100～1 000 mg·L-1范围内,浓度与峰面积线性关系良好,r=0.999 6(n=3).阿奇霉素的平均回收率为100.3%(n=9),日内RSD在0.35%～3.90%之间(n=9),日间RSD在0.35%～4.40%(n=9),重复进样精度RSD%在2%以下(n=5).在pH 3～9之间的溶液中及3%双氧水中,阿奇霉素在12 h内含量基本保持不变.结论:本法简便、迅速、灵敏度高及重现性好,可用于测定阿奇霉素的含量.     

RP-HPLC法测定注射用阿奇霉素有关物质

目的建立注射用阿奇霉素有关物质的新检测方法。方法采用反相高效液相色谱法检测注射用阿奇霉素中有关物质。液相色谱条件为：以Shim-pack CLC-ODS不锈钢柱（250 mm×4.6 mm,5μm）为色谱柱,以0.05 mol·L^-1K2HPO4-乙腈（40∶60）为流动相,流速1.0 ml·min^-1,柱温40℃,检测波长215 nm。结果阿奇霉素有关物质的检测限度为2.5%,阿奇霉素主峰与杂质峰分离完全。结论本方法能简单、灵敏、准确地检测注射用阿奇霉素中的杂质,适用于其有关物质检查。     

HPLC法同时测定阿奇霉素滴眼液中阿奇霉素及苯扎氯铵的含量

目的建立一种高效液相色谱法同时测定阿奇霉素滴眼液中阿奇霉素及苯扎氯铵的含量。方法采用十八烷基硅烷键合硅胶色谱柱(4.6 mm×150 mm,5μm),柱温30℃,以乙腈-磷酸盐缓冲液(取0.05 mol.L-1磷酸氢二钾溶液,用20%磷酸调节pH至8.2)(58∶42)为流动相;检测波长210 nm;流速:1.0 mL.min-1。结果阿奇霉素在1.002 8～5.014 0 mg.mL-1的浓度范围内,苯扎氯铵在6.15μg.mL-1～14.35μg.mL-1的浓度范围内均呈线性。阿奇霉素的平均回收率100.68%,RSD为0.50%(n=9);苯扎氯铵的平均回收率100.59%,RSD为0.92%(n=9)。阿奇霉素与苯扎氯铵的定量限分别为750 ng.mL-1、46 ng.mL-1,平均含量分别为106.94%及100.04%,RSD分别为0.94%及0.67%。仪器重复性RSD值均在2.0%以下。结论本方法简单、准确,可同时测定样品中阿奇霉素及苯扎氯铵的含量。     

阿奇霉素干糖浆联合青霉素治疗小儿急性化脓性扁桃体炎疗效观察

目的 探讨阿奇霉素干糖浆联合青霉素治疗小儿急性化脓性扁桃体炎的临床疗效.方法 治疗组采用阿奇霉素干糖浆5～10 mg·kg-1·d-1,每日1次与青霉素10～20 万u·kg-1·d-1,分2次静脉滴注,连续3 d为1疗程;对照组予以青霉素10～20 万u·kg-1·d-1,分2次静脉滴注,3 d为1疗程.连续1～3个疗程.结果 剔除不合格病例7例(其中4例中途换用或联用其它抗生素,2例流失,1例因药疹停药).进入临床观察病例96例,其中观察组49例,治疗组47例.痊愈率:观察组51%,治疗组66%(P＞0.05);有效率:观察组77.6%,治疗组93.6%(P＜0.05).结论 阿奇霉素干糖浆联合青霉素治疗小儿急性化脓性扁桃体炎安全、方便、疗效显著,值得临床推广.     

微生物比浊法测定口服阿奇霉素的效价含量

目的 建立以微生物比浊法测定口服阿奇霉素效价含量的方法.方法 采用比浊法测定阿奇霉素的含量,并对微生物比浊法、管碟法测定阿奇霉素效价的结果进行评价.结果 阿奇霉素的线性范围为0.4～1.32 u·mL-1(r=0.995 9),分散片与颗粒的平均回收率分别为100.11%,100.27%,方法重复性良好(RSD为0.4%),比浊法与管碟法测定结果一致.结论 微生物比浊法具有简便、精确、快速的特点,可以应用于该产品的质量控制.     

阿奇霉素胶囊溶出度测定方法的改进

目的:以茜素红荷移分光光度法改进阿奇霉素胶囊溶出度的测定方法.方法:依<中国药典>二部附录X C溶出度测定方法项下二法,以600 mL pH 5.0的磷酸盐缓冲液为溶剂,转速为100 r·min-1.经45 min取样,以茜素红荷移分光光度法在524 nm处测定阿奇霉素胶囊的溶出度,限度为75%.结果:阿奇霉素在12.5～62.0 mg·L-1范围内线性关系良好(r=0.991 3),平均回收率为100.3%.结论:该方法准确、简便,可用于阿奇霉素胶囊溶出度的测定.     

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.