复方美愈缓释片的高效液相色谱法分析

目的 :采用反相高效液相色谱法以程序变换控制记录积分衰减因子的方法 ,测定复方美愈缓释片中愈创木酚甘油醚和氢溴酸右美沙芬的含量。方法 :色谱柱为 Shimadzu VP-ODS(15 0 mm× 4.6mm) ,流动相为乙腈 -甲醇 -0 .0 1mol/ L 的三乙胺水溶液 (PH=3 .5 ) (18∶ 15∶ 67) ,检测波长 :2 76nm,流速为 1.0 ml/ m in。结果 :愈创木酚甘油醚和氢溴酸右美沙芬线性范围分别为 5 5 .9～ 782 .6μg/ ml和 4.2～ 5 8.8μg/ ml,平均回收率分别为 98.99% ,RSD1.2 % (n=7) ;10 2 .9% ,RSD 1.6% (n=7)。结论 :该方法可以用于美愈缓释片的含量测定     

反相高效液相色谱法测定人血浆中盐酸二甲双胍的浓度

目的 :以反相高效液相色谱法测定人血浆中盐酸二甲双胍的浓度。方法 :色谱柱为KromasilC18,流动相为0.01mol/LKH2PO4-0 006mol/L -乙腈 (33 5∶33 5∶33) ,流速为1 0ml/min ,检测波长为233nm ,内标为吗啉双胍。结果 :盐酸二甲双胍的线性范围为0 05～4 00μg/ml,回归方程为Y=0 580C +0 0035(r=0 9993) ;日内精密度为2 33 %～8 18% ,日间精密度为0 64%～8 74%。结论 :本方法操作简便 ,测定结果准确 ,重现性好     

高效分子排阻色谱法测定注射用头孢匹胺钠中聚合物的含量

目的:建立高效分子排阻色谱法测定注射用头孢匹胺钠中聚合物的含量。方法:采用TSK-GEL G2000SWXL色谱柱(7.8 mm×300 mm);以磷酸盐缓冲液(p H 7.0)[0.01 mol/L磷酸氢二钠-0.01 mol/L磷酸二氢钠溶液(61∶39)]-乙腈(97.5∶2.5)为流动相;检测波长231 nm;柱温30℃;流速0.8 ml/min;进样量10μl。结果:头孢匹胺在1.962 5~19.624 5μg/ml范围内与峰面积呈良好的线性关系(r=1.000 0),最低检出浓度0.08μg/ml。结论:建立的方法简单、快速、灵敏度高,可有效控制产品的质量。     

HPLC法测定洋金花中东莨菪碱的含量

目的建立洋金花中东莨菪碱含量测定的方法,为提高2005年版药典中洋金花药材的含量测定方法提供标准。方法采用HPLC法测定洋金花中东莨菪碱的含量。色谱柱:ZorbarxC1(250mm×4.6mm,5μm);流动相:0.07mol/L磷酸钠溶液(用磷酸调pH值至6.0,含17.5mmol/L十二烷基硫酸钠)-乙腈(2∶1);流速:0.8ml/min;检测波长:216nm;柱温:25℃;进样量10μl。结果进样量在0.93～9.3μg的范围内线性关系良好,r=0.9999;平均加样回收率为95.8%,RSD%为1.8%。结论该方法精密度高,重复性好,可有效控制洋金花的质量。     

高效液相色谱法测定依达拉奉的含量

目的建立依达拉奉含量的HPLC测定方法。方法采用KromasilC18色谱柱(250×4.6mm,5μm),以甲醇-0.05mol/L磷酸二氢铵溶液(50∶50;用磷酸调pH至3.0)为流动相,流速为0.8ml/min熏检测波长为245nm。结果依达拉奉在10～50μg/ml的浓度范围内呈良好的线性关系穴r=0.9997雪,平均回收率(n=9)为100.10%,RSD=1.3%。结论本方法简便快速,结果准确可靠,可以作为依达拉奉的含量测定方法。     

HPLC法测定天麻素氯化钠注射液中天麻素的含量

目的:建立HPLC定天麻素氟化钠注射液中天麻素的含量.方法:用Hypersil BDS(5μm,4.6mm*250mm)C18柱;以甲醇-0.01mol/L磷酸二氢钠(8:92,磷酸调节pH至4.0±0.1)为流动相;流速0.8ml/min;检测波长220nm;进样量20μl.结果:天麻素在2.5μg/ml～25μg/ml范围内,天麻素浓度与峰面积的线性关系良好(r=0.9998),检测限为1.15ng(S/N=3).回收率为98.9%,RSD=0.08%(n=9).结论:方法简便,结果准确,重复性好.     

HPLC法测定盐酸二甲双胍片的含量

目的建立测定盐酸二甲双胍片含量的方法。方法采用HPLC法,C18柱(250mm×6.0mm,5μm);流动相为0.01mol/L磷酸二氢钾缓冲液(内含0.015mol/L高氯酸,pH为3.0);检测波长为218nm。结果盐酸二甲双胍在8.07～80.74μg/mL浓度范围内线性关系良好(r=0.9991),平均回收率为98.02%,RSD=0.76%。结论本方法简便、快速、准确,专属性强,可作为盐酸二甲双胍片的含量测定方法。     

反相离子对HPLC法测定盐酸二甲双胍中双氰胺的含量

目的建立反相离子对HPLC法测定盐酸二甲双胍中双氰胺含量的方法。方法采用Agilent HC-C18(2)色谱柱(250 mm×4.6 mm,5μm),以甲醇-10 mmol/L庚烷磺酸钠溶液(含0.8%三乙胺,用H3PO4调pH 3.0)(15∶85)为流动相;流速:1.0 mL/min;检测波长:218 nm;柱温:30℃。结果反相离子对HPLC法测定盐酸二甲双胍中双氰胺含量的线性范围为0.01~26.12μg/mL;相关系数r=0.999 9;重复性的RSD为1.8%;精密度RSD为1.6%;高、中、低3种浓度的加样回收率分别为98.8%,102.1%,103.6%;RSD分别为0.8%,1.2%,0.9%。结论此法简便、快速、准确、专属性好。     

HPLC法测定格列齐特片的含量

目的:建立HPLC法测定格列齐特片的含量。方法:采用Diamonsil C18(4.6 mm×250 mm,5μm)色谱柱;流动相0.01 mol/L磷酸二氢钾缓冲液(pH 3.0)-乙腈(30∶70);流速1.5 ml/min;检测波长227 nm,以峰面积计算。结果:线性范围为8~104μg/ml,r=0.999 9。平均回收率为(99.10±1.40)%,RSD为1.41%(n=15)。结论:本方法简便快捷,结果准确,重现性好,可作为格列齐特片质量控制的有效方法。     

HPLC法测定门冬氨酸洛美沙星注射液的含量和有关物质方法研究

目的 :建立高效液相色谱 (HPL C)法测定门冬氨酸洛美沙星注射液的含量和有关物质。方法 :Diamonsil C1 8色谱柱 (2 5 0 mm× 4 .6 mm ,5μm) ,以乙腈 -磷酸盐缓冲液 - 0 .0 5 mol/ L四丁基溴化铵溶液 (19∶ 81∶ 4 )为流动相 ,流速为1.0 ml/ min,用外标法测定 ,检测波长为 2 88nm。结果 :在 16～ 14 4μg/ ml的浓度范围内 ,洛美沙星的浓度与色谱峰面积呈良好的线性关系 ,r=0 .9997;回收率为 99.9% ,RSD=1.2 % ;最低检测量为 2 ng/ ml。结论 :该法准确、简便、灵敏 ,可用于门冬氨酸洛美沙星注射液的含量测定和有关物质检查。     

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.