HPLC法测定可待因甘草合剂中磷酸可待因含量

目的 　建立了用 HPLC法测定可待因甘草合剂中磷酸可待因的含量。 方法 　色谱柱为 ODS (4 .6mm× 2 5 0 mm,5μm) ,甲醇 -0 .0 5 mol·L- 1磷酸二氢钾 (2 0∶ 80 )为流动相 ,流量为 1.0 m L·min- 1 ,检测波长 :2 12 nm。结果 　线性范围 0 .5 19～ 10 .3 80 μg,r=0 .9998,平均回收率为 99.9%(RSD=1.5 2 %,n=9)。 结论 　本法可有效消除甘草合剂对磷酸可待因的干扰 ,结果准确可靠。     

高效液相色谱法测定能量合剂中辅酶A的含量

目的 :建立能量合剂中辅酶A含量测定的HPLC方法。方法 :采用RP -C18(4.6mm× 2 0 0mm ,5 μm)色谱柱 ,以磷酸盐缓冲液 (pH 6 .5 ) -甲醇 (95∶5 )为流动相 ,流速 1.0ml·min-1,检测波长 2 5 9nm ,在室温下对能量合剂中的辅酶A进行含量测定。结果 :辅酶A在 4～ 2 0IU·ml-1的范围内 ,峰面积与效价浓度呈良好线性 (r =0 .9999)。回收率为 10 0 .9% ,RSD为1.8% (n =9)。结论 :该方法简单 ,快速 ,结果准确可靠 ,可作为能量合剂中辅酶A的含量测定方法。     

高效液相色谱法测定结肠安灌肠剂中芍药苷的含量

目的 :应用高效液相色谱法对结肠安灌肠剂中芍药苷进行含量测定。方法 :选用HypersilODS - 2分析柱(2 5 0mm× 4 6mm ,5 μm) ,乙腈 - 0 0 5mol·L-1磷酸二氢钾 (13∶87)为流动相 ,检测波长为 2 30nm ,流速 1 0mL·min-1。结果 :线性范围为 1 12～ 6 72 μg (r =0 99999) ,平均回收率为 97 6 3% ,RSD为 0 85 %。结论 :本法简便、灵敏、准确     

高效液相色谱法测定异烟肼片的含量

目的 　建立 HPL C测定异烟肼片含量的方法。方法 　色谱柱 Kromasil KR10 0 -5 C1 8色谱柱 (2 5 0× 4.6mm) ;流动相 :甲醇 -水 (3 0∶ 70 ) ;流速 :0 .8ml·min- 1 ;紫外检测波长 :2 63 nm。结果 　异烟肼在 0 .2 5～ 2 μg·m L- 1浓度范围内呈线性关系良好。 (r=0 .99999,n=6) ,重复性良好 ,RSD=0 .7% (n=6) ,平均回收率 99.3 3 % ,RSD=0 .64 % (n=6)。 结论 　本法快速、简便、准确、重复性好。     

高效液相色谱法测定小儿运脾合剂中阿魏酸的含量

目的:建立以高效液相色谱法测定小儿运脾合剂中阿魏酸含量的方法。方法:色谱柱为HypersilODS,流动相为0·1%乙酸-甲醇(70∶30),流速为0·8ml/min,柱温为26℃,检测波长为320nm,进样量为20μl。结果:阿魏酸检测浓度在0·02~1·2mg/ml范围内与峰面积积分值线性关系良好(r=0·9997),平均回收率为97·88%(RSD=1·19%)。结论:本方法可用于小儿运脾合剂的质量控制。     

HPLC法测定复方醋酸曲安奈德溶液中两种成分的含量

目的 　建立高效液相色谱法同时测定复方醋酸曲安奈德溶液中两种成分的含量。 方法 　高效液相色谱法 ,选用 Kromasil C1 8柱 ( 5 μm,2 5 0 mm× 4.6mm ) ;流动相。乙腈 -0 .15 %醋酸溶液 ( p H4.0 ,5 3∶ 47,V/V) ;流速 :1.0 ml· min- 1 ;检测波长 :2 40 nm;结果 　曲安奈德与水杨酸分别在 8.18～ 3 2 .7μg· m L- 1 ;15 7.68～ 63 0 .74μg· m L- 1的浓度范围内呈良好的线性关系 ;相关系数分别为 0 .9999和 1.0 0 0 0。平均回收率分别为 10 0 .6%和 10 1.2 % ;RSD分别为 0 .3 %和 0 .4% ( n=9)。 结论 　该方法简便、灵敏、准确、快速。     

高效液相色谱法同时测定复方对乙酰氨基酚维生素C泡腾片中2组分含量

目的 :建立同时测定复方对乙酰氨基酚维生素C泡腾片中对乙酰氨基酚和维生素C含量的高效液相色谱法。方法 :色谱柱 :YWG -C18柱 (10 μm,2 5 0mm× 4 .6mm) ;流动相 :甲醇 乙腈 0 .0 5mol·L-1磷酸二氢铵 磷酸缓冲液 (5 0∶11∶2 5 0 ) ;流速 :1.0mL·min-1;检测波长 :2 5 4nm。结果 :对乙酰氨基酚线性范围为 8～ 16 0mg·L-1;维生素C线性范围为 5～ 10 0mg·L-1。对乙酰氨基酚回收率为 10 0 .4 % (RSD =2 .4 0 % ) ,维生素C回收率为 10 1.2 % (RSD =1.90 % )。结论 :应用本法同时测定对乙酰氨基酚和维生素C含量 ,具有简便、快速、准确、可靠的特点     

HPLC同时测定血清中苯妥英、苯巴比妥和卡马西平的浓度

目的 :建立同时测定微量血清中苯妥英、苯巴比妥和卡马西平浓度的方法。方法 :采用HPLC法 ,以巴比妥为内标同时测定。KromasilC18不锈钢色谱柱 ,流动相为甲醇 水 (5 7∶43) ,流速 0 .8ml·min 1,检测波长 2 5 4nm。结果 :检测浓度范围苯妥英为 4.0～ 5 0 .0 μg·ml 1(r=0 .9995 ) ,苯巴比妥 5 .0～ 6 0 .0 μg·ml 1(r =0 .9996 ) ,卡马西平为2 .5～ 2 0 .0 μg·ml 1(r =0 .9992 )。最低检测限分别为 1.0 μg·ml 1、2 .0 μg·ml 1和 0 .5 μg·ml 1;平均回收率分别为99.2 2 %、99.6 8%和 98.6 2 % ;日内和日间RSD均低于 5 % (n =5 )。结论 :该法准确、灵敏度高 ,重复性好 ,可作为 3种血药浓度监测的常规方法     

高效液相色谱法同时测定血清中苯妥英、卡马西平的浓度

目的 :建立HPLC法同时测定血清苯妥英 (PHT)与卡马西平 (CBZ)浓度。方法 :以C18反相柱为色谱柱 ,甲醇 水 (5 5∶45 )为流动相 ,检测波长 2 40nm ;用乙酸乙酯作为提取剂。结果 :PHT、CBZ平均回收率各为 99.5 %和 10 0 .5 % ,日内和日间RSD均低于 6 .6 % (n =5 ) ;分析方法的定量测定下限 :PHT为 1.2 μ犂·ml-1,CBZ为 0 .2 μ犂·ml-1。分析方法的检测下限 :PHT为 0 .4μ犂·ml-1;CBZ为 0 .1μ犂·ml-1。PHT在 5～ 40 μ犂·ml-1浓度范围线性关系良好 ,r=0 .998;CBZ在 2 .5～ 2 5 μ犂·ml-1浓度范围线性关系良好 ,r=0 .998。结论 :方法灵敏、准确 ,可用于PHT和CBZ临床血药浓度监测。     

离子对色谱法测定心脑安颗粒中葛根素含量

目的 :建立心脑安颗粒葛根素的含量测定方法。方法 :离子对色谱法 ,ODSC18柱 ,4 .6mm× 15 0mm(5 μm) ;流动相 :甲醇 水 (2 0∶80 ) ,内含 0 .0 0 2 4 %磷酸和 0 .0 0 12 %三乙胺 ;检测波长 :2 5 4nm ;流速 :1.0ml·min-1结果 :色谱分离良好 ,在 0 .0 2～0 .6 4 μg范围内成线性关系 ,Y =- 0 .12 5 +2 .6 4 2× 10 -5X ,r =0 .9999,平均回收率为 97.3% ,RSD为 1.5 8%。结论 :本方法简单、快速、准确 ,适合该制剂快速定量分析     

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.