GC法测定法罗培南钠有机溶剂残留量

目的:建立法罗培南钠原料药中有机溶剂残留量测定方法。方法:采用气相色谱法测定,色谱柱为HP-5弹性石英毛细管柱(30 m×0.53 mm,1.5 μm,以5％苯基-95％甲基聚硅氧烷为固定液),进样口温度:200℃,氢火焰离子化检测器(FID),检测器温度:250℃;柱温:程序升温,初始温度35℃,保持5 min,以每分钟10℃的升温速率升温至120℃,保持2 min,再以每分钟35℃的升温速率升温至250 ℃,保持5 min,载气:氮气,流速:2 mL/min,分流比:1:1,尾吹流速:30mL/min,以N-甲基吡咯烷酮为溶剂。结果:待测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度良好。结论:该法可用于法罗培南钠原料药中有机溶剂残留量的检测。     

顶空气相色谱法测定托拉塞米原料药中残留溶剂

目的:检查托拉塞米原料药中甲醇、二氯甲烷、甲苯、二氧六环等有机溶剂残留量。方法:采用气相色谱(GC)法测定,色谱柱为HP-5弹性石英毛细管柱(5%-苯基甲基聚硅氧烷为固定液,30 m×0.53 mm,1μm),进样口温度220℃;氢火焰离子化检测器(FID)温度:240℃;柱温:程序升温,初始温度40℃,保持10 min,以40℃·min-1升温至200℃,保持3 min;载气:N2;流速:5 mL·min-1;以二甲亚砜为溶剂,丙酮为内标物。结果:被测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度良好。结论:该法可用于托拉塞米原料药中有机溶剂残留量检测。     

GC法测定羟苯丙酯中8种有机溶剂的残留量

摘要：目的:建立同时测定羟苯丙酯中甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇、仲丁醇和叔丁醇8种有机溶剂残留量的方法。方法:采用DB-624毛细管柱（0.32 m×30 mm,1.8μm）; FID检测器;进样口温度为200℃,检测器温度为250℃;载气为高纯氮气,载气流速为2.0ml·min-1;柱温为升温程序,起始温度45℃,保持2min,以5℃·min-1升温至65℃保持5 min,再以40℃·min-1升温至200℃保持3 min。结果:羟苯丙酯中8种残留溶剂在各自浓度范围内线性关系良好（r均>0.999）;平均回收率为102.1%～106.2%。结论:本方法操作简单、准确度高、重复性好,可用于羟苯丙酯中8种有机溶剂残留量的测定。     

毛细管气相色谱法同时测定盐酸替利定原料药中4种有机溶剂残留量

目的:建立了以毛细管气相色谱法同时测定盐酸替利定原料药中丙酮、乙酸乙酯、四氢呋喃、甲苯4种有机溶剂残留量的方法。方法:色谱条件为DB-1701毛细管柱,氢火焰离子化检测器,检测器温度为250℃,柱温采用程序升温,初始温度为35℃,保持8min,以30℃·min-1升至180℃,保持2min,进样口温度为155℃,载气为氮气,流速为0.7mL·min-1,分流比为15∶1,进样量为1μL;以二甲基甲酰胺为溶剂。结果:丙酮、乙酸乙酯、四氢呋喃、甲苯的检测浓度线性范围分别为0.100～1.000、0.100～1.000、0.018～0.144、0.0178～0.178mg·mL-1(r为0.9993～0.9999),平均加样回收率为98.2%～99.5%,RSD小于1.5%。3批样品中乙酸乙酯均未检出,丙酮、四氢呋喃、甲苯残留量均符合《中国药典》2005年版要求。结论:本法快速、灵敏、准确,适用于盐酸替利定原料药中有机溶剂残留量的测定。     

毛细管气相色谱法同时检测丙酸氯倍他索原料药中4种有机溶剂残留量

目的:建立丙酸氯倍他索原料药中4种有机溶剂(甲醇、乙醇、N,N-二甲基甲酰胺、二甲亚砜)残留量的检测方法。方法:采用毛细管气相色谱法。色谱柱为HP-INNOWAX石英毛细管柱;溶剂为1,6-二氧六环;程序升温,初始温度60℃,保持5min,并以30℃·min-1速率升温至160℃,保持5min;载气为高纯氮气,流速为1.0mL·min-1;氢火焰离子化检测器温度为250℃;进样口温度为160℃;进样方式为分流进样,分流比为5.0∶1;燃气为氢气,30mL·min-1;助燃气为空气,450mL·min-1;尾吹气为氮气,25mL·min-1;进样量为1μL。在同一条件下检测5批样品中4种溶剂残留量。结果:甲醇、乙醇、N,N-二甲基甲酰胺、二甲亚砜均能达到完全分离,检测浓度线性范围均为0.02～1.0g·L-1(r=1.000);平均回收率为97.6%～102.5%,RSD小于2.88%;最低定量限分别为0.60、0.98、0.38、0.85μg·mL-1;5批样品中有1批检测出甲醇,2批中检测出乙醇,其余均未检测出有机溶剂。结论:该方法灵敏、准确,可同时检测丙酸氯倍他索原料药中4种残留有机溶剂。     

顶空气相色谱法测定依匹必利原料药中有机溶剂残留量

目的:建立以顶空气相色谱法测定依匹必利原料药中3种有机溶剂甲醇、乙醚、三乙胺残留量的方法。方法:采用顶空进样法,以二甲基甲酰胺为溶剂,甲苯为内标,平衡温度70℃,平衡时间30min。气相色谱条件中采用OV1701色谱柱;程序升温:40℃维持2min,以5℃·min-1的速率升至180℃,维持10min;气化室温度为200℃,检测器温度为260℃;载气为氮气,流速为5mL·min-1。结果:甲醇、乙醚、三乙胺检测浓度线性范围分别为53.8～376.6、62.0～434.0、20.2～141.4μg·mL-1(r均>0.9949);回收率均>98.1%,RSD均<1.9%。样品中3种有机溶剂残留量甲醇<0.092%、乙醚<0.0021%、三乙胺<0.00015%。结论:所建立方法灵敏、准确、可靠,适用于依匹必利原料药中有机溶剂残留量的测定。     

氯雷他定原料药中残留溶剂检测方法的研究

建立氯雷他定原料药中有机溶剂残留量测定方法。以Agilent FFAP弹性石英毛细管柱(聚乙二醇为固定液,50 m×320μm×0.5μm)为色谱柱,进样口温度为220℃;氢火焰离子化检测器(FID)温度为240℃;柱温为程序升温,初始温度40℃,保持10 min,以20℃.min-1升温至200℃,保持3 min;载气为氮气,流速3 mL.min-1。此色谱条件下被测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度良好,可用于氯雷他定原料药中有机溶剂残留量检测。     

GC法检测氯法拉滨中有机溶剂的残留量

目的:建立以气相色谱法检测氯法拉滨原料药中7种有机溶剂残留量的方法。方法:毛细管柱为AT-1301;载气为氮气;检测器为火焰离子化检测器;柱温采取程序升温,初始温度40℃,以7℃.min-1升至80℃,再以20℃.min-1升至200℃,保持2min;进样口温度250℃;检测器温度280℃;分流直接进样。检测3批氯法拉滨原料药中甲醇、乙腈、二氯甲烷、叔丁醇、乙酸乙酯、正庚烷、乙酸的残留量。结果:各有机溶剂均能得到有效分离,在所考察的浓度范围内线性关系良好(r=0.99941～0.99993),平均回收率为96.5%～102.4%,RSD均小于4.0%,3批样品中7种有机溶剂残留量均符合《中国药典》要求。结论:本方法灵敏、准确、可靠,可用于氯法拉滨原料药中有机溶剂残留量的检测。     

顶空毛细管气相色谱法测定长春西汀原料药中乙酸乙酯残留量

目的:建立测定长春西汀中残留溶剂乙酸乙酯含量的方法。方法:采用顶空毛细管气相色谱法检测6批长春西汀原料药中乙酸乙酯残留量。以二氧六环为溶剂,丙酮为内标;色谱柱为Ailgent DB-624弹性石英毛细管柱;程序升温:初始温度55℃,保持6 min,并以40℃·min-1的速率升温至180℃,保持2 min;进样口温度200℃,氢火焰离子化检测器检测口温度250℃;氮气流速1.0 mL·min-1;分流进样,分流比为5∶1;顶空温度85℃;平衡时间30 min;进样时间1 min。结果:乙酸乙酯与内标分离良好,乙酸乙酯检测浓度线性范围为0.025～0.25 mg·mL-1(r=0.999 8);加样回收率为102.2%(RSD=1.82%,n=6);最低定量浓度为0.10μg·mL-1。6批样品中只有1批检出乙酸乙酯(0.023%),其余5批均未检出。结论:该法简单、灵敏、准确,可用于长春西汀原料药中乙酸乙酯残留量检测。     

毛细管气相色谱法测定枸橼酸他莫昔芬原料药中有机溶剂的残留量

目的：建立毛细管气相色谱法测定枸橼酸他莫昔芬原料药中有机溶剂残留量的方法。方法：色谱柱：DB-624（30m&#215;0．53mm&#215;3μm）弹性石英毛细管柱；柱温采用程序升温：起始40℃，保持13min，20℃／min升至230℃，保持15min；氢火焰离子化检测器，载气：氮气，流速：3．0ml&#183;min-1，进样口温度：140℃；检测器温度：250℃；分流比为5：1。结果：甲醇、丙酮、乙酸乙酯、四氢呋喃及甲苯浓度的线性均在各自浓度范围内，线性关系良好。平均回收率为：95．1％～98．1％。结论：方法操作简便、结果准确可靠，可以用于枸橼酸他莫昔芬原料药中有机溶剂残留的测定。     

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.     

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.