高效液相色谱法测定塞来昔布胶囊中塞来昔布的含量

目的 　建立测定塞来昔布胶囊中塞来昔布含量的反相高效液相色谱法。 方法 　以美国 Dikma公司 Diamonsil TMC1 8反相柱 ( 2 5 0 mm×4.6mm,5 μm)为色谱柱 ,流动相为甲醇 -超纯水 ( 85∶ 15 ,V/V) ,流速为 0 .8m L· min- 1 ,检测波长 2 5 4nm,柱温 40℃ ,进样量为 5 μL。考察了流动相不同配比对塞来昔布色谱行为的影响。 结果 　塞来昔布与胶囊剂辅料及其杂质可完全分离 ;分析方法的定量测定下限为 2 5μg· m L- 1 ,线性范围 :2 5～ 10 0 0 μg·m L- 1 ,回归方程为 C=1.86× 10 - 2 F+1.84× 10 - 1 ,r=0 .999( n=8) ,平均回收率为 98.2 3 %,RSD=0 .47%。 结论 　该方法灵敏、准确、简单、快速、可用于塞来昔布胶囊的含量测定     

RP-HPLC测定利福昔明的含量及有关物质

目的　建立测定利福昔明含量及有关物质的方法。方法　采用C18色谱柱 (5 μm ,15 0mm× 4.6mm) ,流动相为甲醇 -乙腈 - 0 .0 5mol·L-1磷酸二氢钾溶液 - 0 .5mol·L-1枸橼酸溶液 (5 0∶2 5∶2 0∶5 ) ,检测波长 2 5 4nm。结果　利福昔明在 5 0～ 2 0 0 μg·ml-1浓度范围内 ,峰面积与浓度呈良好的线性关系 (r=0 .9999) ,平均回收率为 99.9%。结论　所建方法简便 ,专属性及重复性好 ,可用于利福昔明的含量及有关物质的测定。     

高效液相色谱法测定美洛昔康胶囊的含量

目的 :建立反相高效液相色谱法测定美洛昔康胶囊中美洛昔康的含量。方法 :采用LichrosorbC18色谱柱 (5 μm,4 .6mm× 2 0 0mm) ,以吡罗昔康为内标 ,甲醇 乙腈 0 .0 9mol·L-1庚烷磺酸钠溶液 冰醋酸 (5 4∶8∶37∶1)为流动相 ,流速为0 .9mL·min-1,检测波长为 35 2nm ,柱温为室温。结果 :美洛昔康在 8～ 4 8mg·L-1范围内呈良好的线性关系 ,r =0 .9999,平均回收率为 99.78% ,RSD为 0 .96 %。结论 :该法简便 ,快速 ,专属性好 ,结果准确 ,可靠。     

离子对高效液相色谱法测定美洛昔康含量及有关物质

目的 :为控制美洛昔康的含量和有关物质 ,建立了离子对高效液相色谱测定法。方法 :色谱柱为Alltech公司AlltimaODS柱 (2 5 0mm× 4 6mm) ,流动相 :乙腈 -含 0 2 5 %辛烷磺酸钠的 0 1mol·L- 1 磷酸二氢钠 (磷酸调至pH 2 5 ) (6 5∶35 ) ,流速 :1mL·min- 1 ,检测波长分别为 35 5nm (含量测定 )和 2 71nm (有关物质测定 )。结果 :美洛昔康在 9～ 110 μg·mL- 1 范围内呈良好的线性关系 ,r=0 9998。结论 :本文改进的离子对高效液相色谱法为测定美洛昔康及其制剂的含量和有关物质提供了可靠基础。     

高效液相色谱法测定更昔洛韦滴眼液的含量

目的 :建立测定更昔洛韦滴眼液含量的高效液相色谱法。方法 :以HypersilC18为色谱柱 ,甲醇 水 (10∶90 )为流动相 ,检测波长 2 5 2nm。结果 :更昔洛韦在 2 .5～ 4 0mg·L-1浓度范围内线性关系良好 (r =0 .9998) ,平均回收率为 10 0 .7% ,RSD为0 .33%。结论 :本方法简便、快速、灵敏 ,可作为该滴眼液的质量控制。     

塞来昔布抑制顺铂致大鼠迟发性呕吐的作用及机制研究

目的:研究选择性环氧合酶-2抑制剂塞来昔布对顺铂致大鼠迟发性呕吐的作用及机制。方法:将大鼠分为对照组、顺铂组和塞来昔布组(顺铂+塞来昔布),各组给予相应药物后观察大鼠摄食高岭土量;测定肠组织中5-羟色胺(5-HT)及其代谢产物5-羟基吲哚乙酸(5-HIAA)含量;测定色氨酸羟化酶(TPH)和单胺氧化酶(MAO)活性;观察小肠黏膜形态学改变。结果:与对照组比较,顺铂组摄食高岭土量明显增加(P<0·05),肠组织内TPH活性增强,MAO活性减弱,5-HT的含量增加(P<0·05)。与顺铂组比较,塞来昔布组摄食高岭土量明显降低,TPH酶活性及5-HT的含量也均降低(P<0·05),且小肠组织病变减轻。结论:塞来昔布可以抑制顺铂所致化疗性异食癖,提示其可能具有防治迟发性恶心、呕吐的作用。     

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     

氢氧化钠溶液呈色的分光光度法测定红霉素片含量

目的 :测定红霉素片的含量。方法 :以 0 .5mol·L-1氢氧化钠溶液为显色剂 ,在 2 36nm波长处测定红霉素片的含量。结果 :红霉素浓度在 2 0 .6 8～ 10 3.4 μg·ml-1范围内呈良好线性关系 (r =0 .9999,n =5 ) ,平均回收率为 10 0 .0 1% ,RSD =0 .91% (n =5 )。结论 :本法简便、准确 ,可用于快速测定红霉素片的含量。     

极谱催化氢波法测定塞来昔布的含量

目的建立一种灵敏快速测定塞来昔布的新方法。方法采用线性单扫描极谱法实现快速测定。结果在0.05 mol.L-1磷酸二氢钾-磷酸氢二钠(KH2PO4-Na2HPO4)缓冲溶液(pH值6.81±0.10)中,塞来昔布于?1.25 V处产生一灵敏的极谱催化氢波,其二阶导数峰电流与塞来昔布浓度在1.0×10-7~2.6×10-6mol.L-1范围内呈线性关系(r=0.997 0,n=6),检出限为5.0×10-8mol.L-1。结论该方法可用于药剂中塞来昔布的测定。     

高效液相色谱-电化学法同时测定多巴丝肼片中2组分含量

目的 :建立高效液相色谱电化学法同时测定多巴丝肼片中左旋多巴 (levodopa,LD)和苄丝肼 (benserazin ,BSZ)的含量。方法 :色谱柱 :SpherisorbODS 2 5 0mm× 4 .0mm柱温 :18℃ ,流动相 :醋酸盐缓冲液 (含柠檬酸 0 .0 3mol·L-1,氢氧化钠0 .0 7mol·L-1,乙酸钠 0 .0 5mol·L-1,用冰醋酸调节 pH至 4 .6 )。流速 :0 .9mL·min-1。电化学检测器 (ECD)。结果 :LD、BSZ的线性范围分别为 0 .2 5～ 10mg·L-1和 0 .0 6 2 5～ 2 .5mg·L-1。LD的回收率为 99.4 %～ 10 2 .4 % ,BSZ回收率为 98.3%～10 1.6 % ,RSD <5 % (n =5 )。LD和BSZ的最低检测浓度分别为 0 .378μg·L-1和 0 .12 4 μg·L-1(S/N >3)。结论 :本法较简便、准确、灵敏度高 ,重现性好     

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.     

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.     

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.     

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.