HPLC法测定苯噻啶含量及其有关物质

本文采用HPLC法测定苯噻啶对照品含量及其有关物质。色谱柱KromasilC18(2 5 0× 4 6mm ,5 μm) ,流动相 :乙腈 -水 -三乙胺 (5 5∶4 5∶0 2 ,磷酸调节溶液pH3 5 ) ,检测波长 :2 5 4nm ,流速 :1 0ml·min-1,进样量 :2 0 μl。苯噻啶在浓度 6 5～ 2 0 8μg·ml-1浓度范围内线性关系良好。回归方程A =64185 74 +81992 3C ,r=0 99998。平均回收率 10 0 1% (n =6) ,RSD为 0 5 8%。本法简便、灵敏、准确     

高效液相色谱法测定苯噻啶的含量

目的　建立苯噻啶含量测定的HPLC方法。方法　选用KromasilC18(2 5 0× 4.6mm ,5 μm)色谱柱 ,乙腈 水 三乙胺 (5 5∶45∶0 .2 )为流动相 ,检测波长 :2 5 6nm ,流速为 1.0mL·mL-1,进样量 2 0 μL。 结果　苯噻啶在浓度为 6.5～ 2 0 8μg·mL-1浓度范围内线性关系良好。回归方程为A =64 185 .74+81992 .3×C ,r=0 .99998。结论　本法简便、灵敏、准确。     

HPLC测定复方阿苯达唑片的含量

目的　用HPLC法测定复方阿苯达唑片中阿苯达唑和双羟萘酸噻嘧啶的含量。方法　采用硅胶柱 ,以乙腈 -混合液[水 -乙酸 -二乙胺 (2 .5∶2 .5∶1) ](5 4∶1)为流动相 ,检测波长 2 88nm。结果　阿苯达唑的线性范围为 0 2～ 0 6 μg ,回归方程为 :Y =1.832× 10 6X +7.2 84× 10 3 (r=0 .9998) ;双羟萘酸噻嘧啶的线性范围为 0 .8～ 2 .4 μg ,回归方程为 :Y =1 2 5 5× 10 6X -1 736× 10 4(r=0 .9995 )。结论　所用方法简便、快速 ,准确、可靠。     

HPLC法测定茵栀黄软胶囊中黄芩苷、栀子苷和绿原酸的含量

目的测定茵栀黄软胶囊中的 3种有效成分 ,黄芩苷、栀子苷、绿原酸的含量。方法HPLC法 ,Irregular HC18(2 5 0 . 0mm× 4 6mm ,10 μm)色谱柱。黄芩苷流动相 :甲醇 水 磷酸 (V∶V∶V =4 7. 0∶5 .3 0∶0. 2 ) ,流速 :1 0mL·min-1,检测波长 :2 80nm ;栀子苷流动相 :乙睛 水 (V∶V =15∶85 ) ,流速 :1 0mL·min-1,检测波长 :2 38nm ;绿原酸流动相 :乙睛 磷酸溶液 (w =0 . 4 % )(V∶V =13∶87) ,流速 :1 0mL·min-1,检测波长 :32 7nm。结果黄芩苷在 2 7 5～ 137 5mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =6 4. 83× 10 4ρ - 1 6. 96× 10 .5 ,r =0 . 9998,平均回收率为 99 4 6 % (RSD =1 0 1% ) ;栀子苷在 16 .5～ 82 . 5mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =8 794× 10 .5ρ - 4 . 116× 10 2 ,r =0 . 9999,平均回收率为 10 0 . 37% (RSD =1 4 .0 % ) ;绿原酸在 2 4～ 12 0mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =2 4 88× 10 4ρ - 9 2 4 4× 10 4,r =0 9999,平均回收率为 99 38%(RSD =1. 89% )。结论测定方法可用于茵栀黄软胶囊的质量控制。     

高效液相色谱法测定卡马西平片的含量

建立卡马西平片含量测定的HPLC方法。色谱柱为LichrosorbDiol (4 0× 2 5 0mm ,5 μm ) ;流动相 :乙腈 -甲醇 - 0 0 5 %冰醋酸溶液 (5∶5∶90 ) ;流速 :1 0ml·min-1;检测波长 :2 30nm ;柱温 :2 5℃ ;峰面积外标法。卡马西平在 10～ 10 0 μg·ml-1范围内具有良好的线性关系 ,回归方程为A =1 6 95 3× 10 4C - 2 5 5 5 5× 10 3 ,r=0 99997;平均回收率为 99 6 9% ,RSD =0 75 % (n =6 )。本法准确可靠 ,专属性强 ,能更好地控制其质量。     

HPLC测定盐酸小檗碱片的含量

目的　建立盐酸小檗碱片的含量测定方法。方法　采用HPLC法 ,选用InertsilODS - 3C18色谱柱 (2 5 0mm× 4 .6mm ,5μm) ,0 .0 33mol·L-1KH2 PO4溶液 -乙腈 (6 5∶35 )为流动相 ,检测波长为 2 6 5nm。结果　盐酸小檗碱在 0 .2～ 1.6 μg·ml-1浓度范围内线性关系良好。回归方程为 :A =4 .2 12× 10 6C - 1.0 0 9× 10 5(r=0 .9999)。结论　所用方法简便、快速 ,结果准确。     

HPLC测定磷酸咯萘啶片中主药的含量

目的　建立测定磷酸咯萘啶含量的HPLC方法。方法　选用DiamonsilC1 8(2 50mm× 4 .6mm ,5μm)色谱柱 ,0 .0 8mol·L- 1 磷酸二氢钾 -乙腈 (85∶1 5)为流动相 (含 0 .1 %三乙胺 ,pH3 .0 ) ;检测波长 2 78nm ;流速为 1 .0ml·ml- 1 ;进样量 2 0 μl。 结果　磷酸咯萘啶在浓度 5 .0 8～ 40 6 .4μg·ml- 1 范围内线性关系良好 ;回归方程为A =- 1 2 91 8+1 8657C ,r =0 .9999;平均回收率为 99.8% ,RSD =0 .8% (n =5)。结论　本法简便、灵敏、准确     

高效液相色谱法测定呱仑酸钠的含量及有关物质

目的 :建立一种用高效液相色谱法测定呱仑酸钠的含量及有关物质的方法。方法 :在InertsilCN - 3柱上 ,以磷酸盐缓冲液 (pH =7) -乙腈 (5 0∶5 0 )为流动相 ,于 2 90nm波长处检测 ,流速为 1 0mL·min-1。结果 :呱仑酸钠的浓度在1 0～ 6 0 μg·mL-1范围内线性关系良好 ,回归方程 :A =6 2 0 0× 10 5C 6 374× 10 4 ,r =0 9996。精密度试验RSD =0 2 9% (n =6 ) ,最低检出限为 0 2 4ng。有关物质可检出 2个杂质。结论 :本方法简单、快速、结果准确     

高效液相色谱法测定盐酸左旋咪唑片的含量

目的　以西咪替丁为内标 ,建立RP -HPLC法测定盐酸左旋咪唑片的含量。方法　选用ODS -C18柱 (5 μm ,4 6mm× 15 0mm) ;流动相 :甲醇 水 二乙胺 磷酸 (36∶6 4∶0 1∶0 0 6 ) ,pH7 0 ;检测波长 :2 15nm ;流量∶1 0ml·min-1;进样体积∶2 0 μl。结果　进样量在 0 32～ 1 6 μg范围内 ,相关性良好 ,回归方程 :Y =2 2 0 1X +7 4× 10 -3 ,r=0 9998。平均回收率为 99 8% (n =5 )。结论　本法简便、快速、准确。     

兔血浆中霉酚酸酯的活性代谢物霉酚酸的HPLC测定及其药代动力学研究

目的建立霉酚酸兔血药浓度测定方法 ,并进行了灌胃后药代动力学研究。方法采用HPLC 二极管阵列检测器测定血药浓度。血样采用乙醚萃取 ;色谱柱 :HypersilODS2 (2 0 0mm×4 6mm ,5 μm) ;流动相 :0 0 5mol·L-1KH2 PO4 CH3 CN(5 5∶45 ,pH 2 5 ) ;检测波长 :2 1 5nm ;流速 :1 0mL·min-1。结果霉酚酸血药浓度线性范围为 0 1 6～ 1 9 98μmol·L-1(r =0 9996,n =8) ,血浆最低检测浓度为 0 0 3 μmol·L-1,高、中、低 3种浓度平均回收率分别为 :(1 0 3 2 5± 6 3 2 ) %、(99 63± 2 75 ) %、(1 0 2 47± 3 1 8) % ,兔灌胃后主要的药代动力学参数分别为 :达峰浓度cmax为(8 2 7± 6 1 2 ) μmol·L-1,达峰时间tmax为 (0 49± 0 1 7)h ,消除半衰期t1/ 2 为 (3 1 2± 0 94)h ,药时曲线下面积AUC0 -t为 (1 3 0 8± 9 0 8) μmol·h·L-1,AUC0 -∞ 为 (1 3 80± 8 93 )mg·h·L-1。结论为霉酚酸的血药浓度监测及药动学研究提供了实验方法。     

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.

     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

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.     

Glycofection: The Ubiquitous Roles of Sugar Bound on Glycoplexes

Glycofection (transfection by using sugar-substituted polylysine) was assessed in order to provide an alternative to viral vectors for the transfer of genes into vascular smooth muscle cells. A rabbit vascular smooth muscle cell line (Rb-1 cells) was selectively transfected by using glycoplexes (glycosylated polylysine/pSV2LUC complexes) in the presence of 10 mu M of the fusogenic peptide GALA. A sugar-specific transfection was obtained when the glycofection was conducted for 1 h with glycoplexes containing either alpha Gal, alpha -Glc, alpha -GalNAc, beta -GlcNAc, or beta -GalNAc residues. The gene expression was high after transfection, with glycoplexes bearing alpha Gal, alpha -GalNAc, or beta -GalNAc residues that were weakly internalized, and low with glycoplexes carrying Lact or Rha residues that were well taken up by cells. These results suggest that 1) glycofection can be a good approach for a selective transfer of genes intovascular smooth muscle cells, 2) an efficient uptake of the glycoplexes is not the unique limiting step for an efficient transfection, and 3) the sugar-dependent trafficking of the glycoplexes inside the cells may account for the transfection efficiency.     

直肠癌下切缘病理组织学分析

目的探讨直肠癌逆向浸润与下切缘的安全距离的关系。方法对36例直肠癌Miles手术和Dixon手术后标本的肿瘤下缘1.0cm、2.0cm、3.0cm的肠壁及对应的系膜病理组织学检查,观察直肠癌逆向浸润或转移的距离。结果36例直肠癌标本距癌肿下缘1.0 cm、2.0cm、3.0cm的肠壁及对应的系膜病理组织学检查均为阴性,结论直肠癌远恻逆向浸润或转移未见超过1.0cm,因此认为保肛手术时切除肿瘤远侧肠管(包括系膜)2.0cm是安全的。