GC测定越橘提取物中的有机溶剂残留量

目的 采用毛细管气相色谱法测定越橘提取物中的甲醇、乙醇、丙酮3种有机溶剂残留量。方法 采用HP-INNOWAX(30 m×0.320 mm,0.50 μm)毛细管色谱柱,氢火焰离子化检测器,程序升温：初始化温度40 ℃(维持6 min),以25 ℃·min^-1速率升温至220 ℃(维持5 min);载气为氮气,进样口温度：220 ℃;检测器温度：250 ℃。结果 3种有机溶剂完全分离,浓度在考察范围内与峰面积具有良好的线性关系,其中甲醇、乙醇、丙酮的线性范围分别为1.035~10.35,10.018~100.18,0.259~2.59 μg·mL^-1,平均回收率分别为97.95%,98.24%,98.10%。结论 本方法灵敏、准确、可靠,能较好地检测越橘提取物中有机溶剂残留量,控制产品质量。     

顶空气相色谱法测定聚普瑞锌中的残留溶剂

目的 建立以顶空气相色谱法测定聚普瑞锌原料药中甲醇、乙醇、三氯甲烷和甲苯4种有机溶剂残留量的方法。方法 以1 mol·L^-1硫酸溶液为溶剂,采用Agilent DB-FFAP(30 m×0.32 mm,0.5 μm)毛细管柱,载气为氮气,柱流速为2 mL·min^-1;柱温为程序升温,氢火焰离子化检测器(FID),检测器温度为250 ℃;进样口温度为200 ℃;顶空瓶平衡温度为80 ℃。结果 甲醇、乙醇、三氯甲烷和甲苯均能较好的分离,呈现良好的线性关系,平均回收率分别为102.9%,105.4%,93.8%,95.7%,RSD分别为2.9%,2.1%,3.3%,3.5%(n=9)。结论 本方法简便快速,准确性好,灵敏度高,可用于聚普瑞锌原料药中残留溶剂的测定,同时也为难溶性原料药中的残留溶剂测定提供一个思路。     

GC同时测定利伐沙班原料药中7种有机溶剂残留

目的 建立以毛细管气相色谱法测定利伐沙班原料药中乙醇、二氯甲烷、四氢呋喃、三乙胺、吡啶、乙酸、N,N-二甲基甲酰胺(DMF)7种有机溶剂残留量的方法。方法 采用Agilent DB-624(30.0 m×0.32 mm,1.8 μm)毛细管柱,载气为氮气,采用氢火焰离子化检测器(FID),进样口温度为200 ℃,检测器温度为240 ℃,柱温采用程序升温,流速为2.0 mL·min^-1,进样量1 μL。结果 无水乙醇、二氯甲烷、四氢呋喃、三乙胺、吡啶、乙酸、DMF均能得到较好的分离,呈现良好的线性关系,平均回收率分别为102.4%,100.1%,96.5%,91.6%,103.6%,106.6%,102.5%,RSD均<5.0%。结论 本方法简便、快速、准确性好、灵敏度高,可用于利伐沙班原料药中残留溶剂的测定。     

顶空气相色谱法测定阿奇霉素中的有机溶剂残留量

摘 要 目的: 建立测定阿奇霉素原料药中甲醇、乙醇、甲苯等3种有机溶剂残留量的顶空气相色谱法。方法: 分析柱为DB 624毛细管柱(30 m×0.53 mm,3 μm),载气为高纯氮气,流速为1.0 ml·min^-1,进样口温度为200℃,柱温为程序升温,初始温度为40℃,保持2 min,以15℃·min^-1的速度升温至150℃,再以20℃·min^-1的速度升温至200℃保持8 min,检测器为FID,检测器温度为250℃,顶空恒温箱温度为95℃,平衡时间为30 min。结果: 甲醇、乙醇、甲苯的线性范围分别为6.026～449.175 μg·ml^-1,2.469～757.650 μg·ml^-1,0.551～142.200 μg·ml^-1,平均回收率分别为98.03%,96.62%,97.17%,RSD分别0.42%,0.38%,0.60%（n=9)。结论: 该法简便,准确,其他组分不干扰测定,可用于测定阿奇霉素中的有机溶剂残留量。     

GC测定甲苯咪唑中的残留溶剂

目的 采用顶空气相色谱法测定甲苯咪唑原料药中的有机溶剂残留量。方法 以DMF-H₂O（2︰1）溶液为样品溶剂,选用PerkinElmer气相色谱仪,配备顶空进样器和FID检测器,Agilent DB-624毛细管柱为分析柱,外标法测定。结果 甲醇、乙醇、异丙醇、三氯甲烷和甲苯分别在18.7~224,46.9~562,46.9~562,1.50~17.9,2.81~33.8 μg·mL^-1内线性关系良好（r>0.999）;各组分检出限分别为0.19,0.10,0.11,0.18,0.08 μg·mL^-1;各组分回收率为90.0%~110.0%。结论 该方法准确、灵敏、可靠,可用于甲苯咪唑有机残留溶剂的测定。     

顶空气相色谱法测定左卡尼汀原料药中三甲胺的含量

目的 建立了气相色谱法准确测定左卡尼汀原料药中三甲胺的检测方法。方法 采用程序升温法,FID检测器,色谱柱为Pora PLOT Amines毛细管柱(25 m×0.32 mm×10 μm)进行测定。结果 在选定的测定条件下,三甲胺在0.081 6~4.079 7 μg﹒mL^-1范围内与峰面积呈良好的线性关系,相关系数为0.999 1,平均回收率为99.6%（RSD=1.9%）,检测限为0.025 0 μg﹒mL^-1。结论 该气相色谱方法准确,灵敏度高,可用于左卡尼汀原料药中三甲胺的质量控制。     

离子液体-顶空气相色谱法检测酮康唑中的多种高沸点有机残留溶剂

目的 建立酮康唑原料药中有机溶剂残留量检测的高灵敏方法,初步探索有机溶剂与离子液体(ILs)之间相互作用规律,为选择合适的ILs作为顶空溶剂进行残留测定提供依据。方法 精密称取原料药0.01 g,置10 mL顶空瓶中,精密加入1 mL ILs,密封,微波功率150 W辐射75 s溶解后,置110 ℃恒温箱中平衡30 min,抽取顶部空气1 mL,进气相色谱仪(GC)分析检测,考察并优化顶空溶剂。采用ZB-1毛细管柱(100%二甲基聚硅氧烷, 0.53 mm×60 m,5 μm),FID检测器,程序升温。结果 乙醇、二氯甲烷、乙酸乙酯、正丁醇、吡啶、N,N-二甲基甲酰胺、二甲基亚砜分离度良好,分别在1.25~200,1.50~24.0,12.5~200,12.5~200,0.500~8.00,2.20~3.52,12.5~200 mg·L^-1内线性关系良好,平均回收率在89.8%~98.2%内,RSD均<4.0%。对于乙醇,ILs的顶空效率随着阳离子烷基链的增长而增加,对于乙酸乙酯、DMF和DMSO,ILs的顶空效率随阳离子烷基链的增长而降低,而阴离子对ILs的顶空效率影响相对较小,最终确定[Bmim][PF6]为最佳顶空溶剂。结论 该方法简单、快速、灵敏度高,适用于同时测定酮康唑原料药中多种有机溶剂残留,为药物中高沸点有机残留溶剂的检测提供了一种新手段。对于质子性溶剂,ILs的顶空效率随阳离子极性的减小而增加,对于具有亲质子能力的非质子性溶剂,ILs的顶空效率随阳离子极性的减小而降低,而阴离子的极性对ILs顶空效率影响较小,为选择合适的ILs作为顶空溶剂进行残留测定提供参考依据。     

GC测定甘氨酸原料药中12种有机溶剂的残留量

目的 建立同时测定甘氨酸原料药中甲醇、乙醇、丙酮、异丙醇、乙腈、二氯甲烷、正丙醇、乙酸乙酯、四氢呋喃、环己烷、正丁醇和甲苯12种有机溶剂残留量的方法。方法 采用DB-624毛细管柱（30 m×0.53 mm,3.0 μm）程序升温,氢火焰离子化检测器（FID）,进样口温度为150℃,检测器温度为250℃,载气为高纯氮气,载气流速为2.2 mL·min^-1,分流比为10∶1,顶空加热温度为80℃,平衡时间为35 min。结果 甘氨酸中12种残留溶剂在各自质量浓度范围内与峰面积线性关系良好（r均>0.999）;精密度、稳定性试验的RSD均<5%,重复性试验中只检出乙醇、丙酮、异丙醇（RSD≤1.8%）;平均加样回收率为97%~102%。结论 该方法操作简单、快速灵敏、结果准确,可用于甘氨酸原料药中12种有机溶剂残留量测定。     

氢溴酸沃替西汀原料药中催化剂钯残留监测方法建立

目的：建立氢溴酸沃替西汀原料药中催化剂钯的残留量测定方法。方法：采用石墨炉原子吸收分光光度法测定氢溴酸沃替西汀中钯的残留量。试验条件：光源为钯空心阴极灯,波长247.6 nm,狭缝0.4 nm,灯电流2 mA,石墨管为横向加热方式,石墨炉程序升温。结果：钯浓度在0~80 μg·L^-1与吸光度呈良好的线性关系y=0.003x-0.001（r=0.9995）,检测限为0.59 μg·L^-1,定量限为1.96 μg·L^-1;平均回收率为102.1%,RSD为3.24%（n=9）。结论：该方法经方法学验证,可用于氢溴酸沃替西汀原料药中钯含量的测定,可为该原料药质量标准的建立提供依据。     

顶空进样-毛细管气相色谱法测定格列美脲原料药中5种溶剂残留的含量

目的:建立采用顶空进样—毛细管气相色谱法对第3代治疗糖尿病药物磺酰脲类降糖药格列美脲原料药中正己烷、丙酮、二氯甲烷、甲醇和甲苯5种有机溶剂的残留量测定方法,为格列美脲原料药中5种有机溶剂的残留量提供科学检测方法。方法:采用顶空进样程序升温法,平衡温度为110℃,FID检测器,DM-5毛细管色谱柱(30m×0.32mm,0.25μm)进行检测。结果:5种有机溶剂在各自浓度范围线性关系良好(r=0.9958~0.9991,n=5),最低检测限为0.58~11.8μg·ml-1;定量限范围为1.9~47.3μg·ml-1;3个浓度的平均回收率为95.1%~103.5%,(RSD=1.0%~5.1%,n=6)。结论:该方法灵敏简单、科学严谨、可操作性强、结果可靠,可用于实际生产格列美脲原料药中5种溶剂残留的测定分析。     

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.     

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.     

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.