高效液相色谱法测定复方曲马多片含量

目的 :应用高效液相色谱法测定复方曲马多片含量。方法 :采用KromasilC18 柱 ,以非那西丁为内标 ,甲醇 -水 -三乙胺(55∶45∶0 2)为流动相 (冰醋酸调pH至4 2) ,检测波长为267nm ,流速0 7ml/min。结果 :曲马多线性范围为50～500μg/ml(r=0.9999 ,n=5) ;奈福泮线性范围为50～500μg/ml(r=0 9999 ,n=5)。曲马多平均回收率为99.69 % ,含量测定结果为100 71 % ,RSD=0.76 % (n=5) ;奈福泮平均回收率为99.76 % ,含量测定结果为99.64 % ,RSD=0.62 % (n=5)。结论 :本方法简便、快速、灵敏 ,结果准确。     

高效液相色谱法测定复方氨酚苯海拉明片中对乙酰氨基酚和咖啡因的含量

目的建立一种快速、准确的高效液相色谱法测定复方氨酚苯海拉明片中对乙酰氨基酚和咖啡因含量的方法。方法色谱柱HypersilODS2(5μm,250mm×4.6mm)流动相:甲醇-水(30∶70);流速:1mL.m in-1;检测波长:280nm;柱温:室温;进样量:20μL。结果对乙酰氨基酚进样量在1.50μg~9.00μg范围内线性良好,r=0.99999。平均回收率为99.97%,RSD=0.51%(n=9);咖啡因进样量在0.15μg~0.90μg范围内线性良好,r=0.99999(n=9)平均回收率为99.79%,RSD=0.99%(n=9)。结论试验结果表明本法简便快速,重现性好,结果准确可靠,可以作为复方氨酚苯海拉明片中对乙酰氨基酚和咖啡因的含量测定的方法。     

RP-HPLC法测定野菊花注射液中绿原酸和咖啡酸的含量

目的:建立了同时测定野菊花注射液中绿原酸和咖啡酸含量的方法。方法:采用 RP-HPLC 法,C_(18)柱(250mm×4.6mm,5μm),流动相为乙腈-水-磷酸(12∶88∶0.04),检测波长为327nm。结果:绿原酸与咖啡酸分别在2.0～20.0μg·mL~(-1)(r=0.9997)和0.2～2.1μg·mL~(-1)(r=0.9998)内与峰面积呈良好的线性关系(n=6),方法回收率(n=9)分别为101.4%和99.4%,RSD 分别为1.5%,2.6%。结论:方法简便、快速、准确,重现性好,可用于野菊花注射剂中绿原酸和咖啡酸含量的同时测定。     

HPLC法测定吴茱萸超微速溶饮片中吴茱萸碱、吴茱萸次碱及柠檬苦素的含量

目的建立一种同步测定吴茱萸超微速溶饮片中吴茱萸碱,吴茱萸次碱及柠檬苦素含量的高效液相色谱方法。方法采用Hypersil ODS2C18柱(4.6mm×250mm,5μm),岛津LC-20AD高效液相色谱仪,流动相为乙腈-水-四氢呋喃-冰醋酸(34:64.7:1.1:0.2),流速:1.0mL/min,检测波长:225nm,柱温:30℃。结果吴茱萸碱、吴茱萸次碱、柠檬苦素进样量分别在0.1016～2.032μg(r2=0.9999,n=6)、0.0974～1.948μg(r2=0.9999,n=6)、0.7010～14.02μg(r2=0.9999,n=6)范围内与峰面积呈良好线性关系,平均回收率分别为100.37%(RSD=1.29%,n=6)、99.11%(RSD=0.83%,n=6)、99.30%(RSD=0.52%,n=6)。结论该测定方法简便,测定结果准确,重复性好,可作为质量控制方法。     

HPLC法测定蒿甲醚注射液的含量

目的:建立蒿甲醚注射液含量测定的高效液相色谱方法。方法:采用 Alltima C_(18)柱(150 mm×4.6 mm,5μm),以乙腈-水(70:30)为流动相,流速为1.0 mL·min~(-1),外标法测定,检测波长为210 nm。结果:线性范围为190～3800μg·mL~(-1),r=0.9999;平均回收率(n=3)分别为99.2%(RSD=0.68%),99.6%(RSD=0.55%),99.6%(RSD=0.18%);最低检测限为1.14μg;最低定量限为3.05μg。结论:该法准确、简便,适用于蒿甲醚注射液的含量测定。     

HPLC法测定维格列汀片中的有关物质

目的:建立测定维格列汀片中有关物质的方法。方法:采用高效液相色谱法。色谱柱为Xterra MS C_(18),流动相为[磷酸盐缓冲液-水-乙腈-甲醇(400∶600∶15∶15,V/V/V/V)]-[磷酸盐缓冲液-乙腈-甲醇(400∶450∶150,V/V/V)](梯度洗脱),流速为1.2mL/min,检测波长为210 nm,柱温为35℃,进样量为10μL。结果:杂质A、B、C、D检测质量浓度线性范围分别为18.80~188.0μg/mL(r=0.999 5)、22.64~226.4μg/mL(r=0.999 6)、21.74~217.4μg/mL(r=0.999 7)、19.12~191.2μg/mL(r=0.999 8);检测限分别为4.18、2.68、1.12、1.34μg/mL;精密度、稳定性、重复性试验的RSD<3%;加样回收率分别为97.9%~103.1%(RSD=2.01%,n=9)、98.8%~104.1%(RSD=1.93%,n=9)、98.0%~103.6%(RSD=1.81%,n=9)、100.8%~104.1%(RSD=0.98%,n=9)。结论:该方法操作简单、结果准确,可用于维格列汀片中有关物质的测定。     

HPLC法同时测定苦参碱葡萄糖注射液中苦参碱及有关物质的含量

目的:建立高效液相色谱法测定苦参碱葡萄糖注射液中苦参碱及有关物质的含量。方法:以 Lichospher 氨基柱(200mm×4.6mm,5μm)为分离柱;乙腈-0.02 mol·L~(-1)磷酸二氢钠(75:25)为流动相;流速:1.0mL·min~(-1);检测波长:210nm;进样量:20μL。结果:采用该方法线性范围为0.006～0.40mg·mL~(-1)(r=0.9990,n=6);稳定性试验 RSD 为0.43%(n=5);重复性试验 RSD 为0.52%(n=5);平均回收率为100.7%(n=9)。结论:本法简便、准确,重复性好,可用于苦参碱葡萄糖注射液的质量控制。     

HPLC法同时测定酚氨咖敏颗粒中三组分的含量

目的:建立 HPLC 法同时测定酚氨咖敏颗粒中对乙酰氨基酚、咖啡因、氨基比林的含量。方法:采用日本岛津 VP-ODS色谱柱(150 mm×4.6 mm,5μm),以甲醇-水(40:60)为流动相,流速:1.0 mL·min~(-1),检测波长273 nm,柱温:30℃,进样量:20 μL。结果:对乙酰氨基酚进样浓度在10～100μg·mL~(-1)范围内线性关系良好(r=0.9999),平均回收率(n=3)为98.8%～99.4%;咖啡因进样浓度在2.4～24μg·mL~(-1)范围内线性关系良好(r=0.9999),平均回收率(n=3)为98.2%～101.5%;氨基比林进样浓度在8～80μg·mL~(-1)范围内线性关系良好(r=0.9998),平均回收率(n=3)为98.3%～100.4%。结论:本方法灵敏度高,操作简便、可靠,适用于测定酚氨咖敏颗粒中对乙酰氨基酚、咖啡因、氨基比林的含量。     

RP—HPLC法测定羧胺三唑含量及有关物质

目的:采用反相高效液相色谱法测定羧胺三唑的含量及其有关物质。方法:采用Kromasil C_(18)色谱柱(4.6mm×250mm,5μm);以乙腈-水相(45∶55)为流动相;流速2.0mL·min~(-1);检测波长:262nm;柱温:室温;进样量:20μL。结果:反相高效液相色谱法测定的线性范围为12.5～200μg·mL~(-1);相关系数r=0.9999;日内精密度:RSD为0.38%(n=5);日间精密度:RSD为0.39%(n=5)。结论:本法简便快速、准确、专属性好。     

复方替硝唑含漱液中替硝唑与盐酸达克罗宁的含量测定

目的:建立测定复方替硝唑含漱液中替硝唑与盐酸达克罗宁含量测定的方法。方法:紫外分光光度法,采用倍率系数法与等吸收消去相结合的方法。结果:替硝唑和盐酸达克罗宁的线性范围分别为4～20μg·ml~(-1)(r=0.9999);4～20μg·ml~(-1)(r=0.9999)加样回收率分别为100.4%,RSD=0.66%及100.7%,RSD=0.64%(n=5)。结论:紫外分光光度法可用于本制剂的含量测定和质量控制,方法简便,结果准确。     

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.