GC-MS/MS测定头孢拉定原料中N,N-二甲基甲酰胺及N-甲基乙酰胺的残留量

摘要：目的:建立GC-MS/MS测定头孢拉定原料中N,N-二甲基甲酰胺（DMF）及N-甲基乙酰胺（NMAC）的残留量的方法。方法:色谱条件Agilent VF-WAXms毛细管柱（30 m×0.25 mm, 0.25μm）,进样口温度为250℃;载气为高纯氦气,进样口为恒流模式,流速1.0 ml·min-1;分流进样,分流比10∶1。程序升温:初始温度50℃,保持1min,以10℃·min-1的速率升至180℃,保持2 min,再以20℃·min-1的速率升至240℃,保持10 min。质谱条件离子源为电子轰击源（EI）,离子源温度280℃。碰撞气为氮气,流速1.5 ml·min-1。质谱传输接口温度250℃。质谱监测模式为多反应监测（MRM）。结果:DMF在0.109～7.270μg·ml-1内与其峰面积呈良好的线性关系（r=0.999 9）,加标回收率为92.70%（RSD=4.28%,n=6）;NMAC在0.109～7.280μg·ml-1内与其峰面积呈良好的线性关系（r=0.999 9）,加标回收率为109.89%（RSD=4.24%,n=6）。结论:本方法经方法学验证,可用于测定头孢拉定中DMF及NMAC的残留量。     

毛细管气相色谱法检测水皂角等中药提取物有机氯农药残留

目的:建立水皂角等中药提取物中六六六及滴滴涕异构体含量的气相色谱分析方法。方法:样品采用改进了的微量化学法进行提取,浓硫酸净化,以不分流方式进样,用HP-5弹性石英毛细管柱分离样品,微电子捕获检测器检测,载气为高纯氮气,流速为1.5 mL·min-1,尾吹速度为40 mL·min-1,进样口温度250℃,检测器温度300℃。柱初始温度为100℃,以20℃·min-1升至160℃后,保持2 min,以10℃·min-1升至250℃,保持6 min。结果:最小检测量为1.4×10-14-1.2×10-12g,加样平均回收率为93.2％-101.6％;被测样品中均含有不同程度的有机氯农药残留。结论:该法快速、灵敏、准确,各项技术指标均满足农药残留检测的要求。     

GC法测定甲基纤维素中甲氧基的含量

目的:建立毛细管柱GC法测定甲基纤维素中甲氧基含量的方法.方法:通过氢碘酸与甲基纤维素中的甲氧基反应生成挥发性的碘甲烷,通过GC法测定碘甲烷来计算甲基纤维素中甲氧基的含量.采用DB-624石英毛细管柱(30 m×0.53 mm×3.0μm);氢火焰离子化检测器,柱温为程序升温,100℃保持10 min,然后以50℃·min-1升至230℃,保持2 min;进样口温度200℃,检测温度250℃,载气为氮气;流速为3.0 mL·min-1.以正辛烷为内标物,内标法定量.结果:甲氧基在2.19～19.38 g·L-1浓度范围内与峰面积呈良好的线性关系(γ=0.999 7,n=7),回收率99.3%(RSD=1.14%,n=9).分析了4批样品,甲氧基的含量为29.66%～30.31%.结论:本法专属性强、简便、准确,为更好地控制甲基纤维素的质量提供了切实可行的方法.     

艾拉莫德原料药中残留溶剂检测方法的研究

目的:检查艾拉莫德原料药中的有机溶剂残留量。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(以5％苯基-95％甲基聚硅氧烷为固定液,1.5μm,30 m×0.53 mm);进样口温度:200℃;氢火焰离子化检测器(FID),检测器温度:300℃;柱温:程序升温,初始温度30℃,保持13 min,以5℃·min-1升温至35℃,保持7 min,再以10℃·min-1升温至230℃,保持5 min;载气:氮气;流速:1.5 mL·min-1;以N-甲基吡咯烷酮为溶剂,正丙醇为内标物。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:该法可用于艾拉莫德原料药中有机溶剂残留量检测。     

乳糖与盐酸氟西汀(仲胺)的美拉德反应

最早科学家认为只有芳香伯胺可发生美拉德反应,后来研究表明几乎所有芳香族,脂肪族伯、仲胺均可发生美拉德反应。本文主要讨论乳糖-氟西汀体系中的美拉德/Amadori反应。实验部分　GC/MS:MicroMassTRIO型,四极杆质谱,EI源,气体扫描5min,解吸5min,GLT解吸温度:初温100℃,40℃·min-1升温至200℃,低温阱-100℃;HP5890型GC:进样口温度150℃,传输线温度300℃,分流流速7或50mL·min-1,低温阱迅速加热至250℃使样品解吸入色谱柱,炉温40℃保持3min,10℃·min-1升温至300℃,保持3min,色谱柱DB-1,30m×0.25mmid,1.0mm膜厚。HPLC:SP8700×R…     

野菊花注射液的GC指纹图谱

目的建立野菊花注射液GC指纹图谱。方法使用DB-17弹性石英毛细管柱(30 m×0.25 mm,0.25μm)。柱温:初温80℃保持5 min,以5℃.min-1升至100℃保持10 min,5℃.min-1升至170℃保持5 min,10℃.min-1升至250℃保持3 min;载气:高纯氮气,流量,1.0 mL.min-1;分流比10∶1;氢气:40 mL.min-1;空气:400 mL.min-1;检测器:FID;检测器温度:280℃;气化室温度:280℃;进样量:1μL。结果建立了野菊花注射液的对照指纹图谱并确定了22个共有峰,各批注射液与对照指纹图谱相似度均在0.95以上。结论该方法简便、准确、重现性好,为野菊花注射液的质量控制提供了依据。     

GC/MS法同时检测生物样品中苯丙胺、甲基苯丙胺及MDMA

目的:建立体液和组织中苯丙胺、甲基苯丙胺和3,4 -亚甲基二氧基甲基苯丙胺(MDMA)的简便快速、灵敏可靠的GC/MS检测方法。方法:样品经碱化,乙醚提取,TFA衍生化后,GC/MS全扫描定性检测,选择离子扫描(SIM)定量分析。结果:几种药物在血浆中的线性范围为0 .0 2 - 2 . 0 μg·ml-1,最低检出浓度为0 . 0 0 5 μg·ml-1(S/N≥3) ;肝脏中线性范围为0 . 0 5 - 5. 0 μg·g-1,最低检出浓度0. 0 .10 μg·g-1(S/N≥3)。相关系数大于或等于0 9980 ;回收率在92. 1% - 10 5. 2 %之间。结论:GC/MS方法适用于生物样品中苯丙胺、甲基苯丙胺和MDMA浓度的检测。     

毛细管气相色谱法测定海狗油胶丸中ω-3多不饱和脂肪酸的含量

目的:用毛细管气相色谱法测定海狗油中二十碳五烯酸(EPA)、二十二碳五烯酸(DPA)和二十二碳六烯酸(DHA)的含量。方法:采用HP-INNOWAX毛细管柱(30 m×0.320 mm,0.25 μm),柱温150℃,保持5 min后,以10℃·min-1升至200℃后,继续以5℃·min-1升至240℃,保持7 min,载气为氮气(99.999％)。进样口温度为240℃,检测器温度为270℃,FID检测器。结果:EPA甲酯平均回收率为99.5％,RSD为1.2％;DPA甲酯平均回收率为98.8％,RSD为1.1％;DHA甲酯平均回收率为98.5％,RSD为0.9％。结论:此法操作简单、准确,重复性、稳定性好,是一种可行的ω-3多不饱和脂肪酸含量测定方法。     

GC法同时测定鱼腥草注射液中4种成分的含量

目的:建立同时测定鱼腥草注射液中4-萜烯醇、α-松油醇、乙酸龙脑酯和甲基正壬酮含量的方法.方法:采用气相色谱法;色谱柱:DB-1毛细管气相色谱柱(30m×0.25 mm,0.25μm);程序升温:70℃保持5 min,以5℃·min-1上升至140℃,保持5 min,再以20℃·min-1升至250℃;进样口温度:25...     

羌活和独活药材气相色谱指纹图谱的建立及鉴别

目的为羌活和独活药材的鉴别提供科学依据。方法采用气相色谱(GC)-氢火焰离子化检测法。色谱柱:DB-1毛细管柱(30 m×0.25 mm×0.25μm);程序升温:起始柱温50℃,8℃.min-1升至85℃保持12 min,4℃.min-1升至155℃保持18 min,12℃.min-1升至250℃保持5 min;气化室温度:250℃;载气:氮气;流速:1.2 mL.min-1;进样量:1.0μL;分流比:10∶1;检测器温度:270℃。结果建立了羌活和独活药材的GC指纹图谱;对不同产地药材分别进行了相似度计算;指纹图谱和相似度计算结果显示,羌活和独活药材挥发油含量具有明显区别。结论本方法可用于羌活和独活药材的定性鉴别。     

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.