共查询到20条相似文献,搜索用时 62 毫秒
1.
目的 建立气相色谱法测定氧氟沙星和诺氟沙星中N-甲基哌嗪和哌嗪的残留量的方法。方法 采用Agilent HP CAM 毛细管色谱柱(30.0 m×0.25 mm,0.25 μm);进样口温度为230 ℃;FID检测器温度为280 ℃;柱温:程序升温,70 ℃保持3 min,然后以40 ℃·min-1的速率升温至180 ℃,保持2 min;以氮气为载气,流速为2.0 mL·min-1;直接进样,进样量为0.2 μL;以水为溶解介质,以吡啶为内标,测定了氧氟沙星和诺氟沙星中N-甲基哌嗪和哌嗪的残留量。结果 N-甲基哌嗪、哌嗪与内标均能良好分离,线性范围分别为10.09~201.88 μg·mL-1(r=0.999 6),10.08~201.60 μg·mL-1(r=0.999 5)。结论 该方法重复性良好,回收率符合规定,适用于氧氟沙星和诺氟沙星中N-甲基哌嗪和哌嗪残留量的测定。 相似文献
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目的 建立氢溴酸替格列汀中遗传毒性杂质溴乙烷残留量的气相色谱(GC)检测方法。方法 采用迪马DM-624色谱柱(30 m×0.53 mm×3.0 μm);电子捕获检测器(ECD);程序升温:初始柱温40 ℃,保持3 min,以20 ℃/min升温至200 ℃,保持5 min;进样口温度:210 ℃;检测器温度:210 ℃;载气:氮气;分流比:3:1;进样量1 μL。结果 溴乙烷在0.75~6.75 μg/mL与峰面积呈良好的线性关系(r=0.999 7),最低检测限为0.26 μg/mL。平均回收率为99.4%,RSD值为0.3%(n=9)。3批氢溴酸替格列汀样品中均未检测出溴乙烷。结论 该方法简便、准确,重复性好,适用于氢溴酸替格列汀中溴乙烷残留量的控制。 相似文献
3.
GC法测定小儿氨酚烷胺颗粒中盐酸金刚烷胺 总被引:1,自引:0,他引:1
目的 建立GC法测定小儿氨酚烷胺颗粒中盐酸金刚烷胺。方法 采用HP-5毛细管柱(30 m×0.32 mm×0.25 μm),FID检测器;气化室温度为220 ℃,检测室温度为300 ℃。采用程序升温,初始温度为70 ℃,以10 ℃/min升至140 ℃。载气:氮气,流速为4 mL/min;进样量为1 μL;分流比:1:50。采用内标法定量。结果 盐酸金刚烷胺在0.1~0.7 mg/mL线性关系良好(r=0.999 6)。平均回收率为99.27%,RSD值为0.66%(n=9)。结论 本法简便、准确、重复性好,可用于小儿氨酚烷胺颗粒中盐酸金刚烷胺的测定。 相似文献
4.
GC测定克痢痧胶囊中的冰片、甲基丁香酚和丁香酚的含量 总被引:1,自引:1,他引:0
目的 采用GC测定克痢痧胶囊中的冰片、甲基丁香酚和丁香酚的含量。方法 采用GC直接进样,色谱柱为AgilentHP-INNOWAX毛细管柱,检测器为氢火焰离子化检测器,温度为250℃,采用程序升温,进样口温度为210℃;流速为1.2 mL·min-1,分流比为15︰1,进样量为1 μL。结果 冰片、甲基丁香酚和丁香酚的线性范围分别是48.59~728.88 μg·mL-1(r=0.999);4.29~64.39 μg·mL-1(r=0.999)和31.83~477.48 μg·mL-1(r=0.999),精密度、重复性和稳定性试验的RSD均≤2.17%,平均加样回收率分别是98.69%(RSD=0.3%),93.10%(RSD=1.6%)和99.41%(RSD=0.5%)。结论 本方法操作简单、快速、准确性和重复性好,可用于克痢痧胶囊的质量控制。 相似文献
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目的 建立气相色谱(GC)法测定异环磷酰胺原料药中3种有关物质(起始物料3-氨基丙醇、杂质D和杂质F)。方法 采用HP-55% Phenyl Methyl Siloxane色谱柱(30 m×320 μm,0.25 μm);采用程序升温的方式,起始柱温50℃,保持2 min后以每分钟5℃的速率升温至180℃,再以每分钟20℃的速率升温至260℃;进样口温度为380℃;检测器温度为380℃;分流比5∶1。结果 起始物料峰、杂质D、杂质F与周围峰分离度分别为2.6、3.0、1.6;异环磷酰胺起始物料3-氨基丙醇在39.80~199.0 μg·mL-1线性关系良好(r=0.999 1),杂质D在39.48~197.4 μg·mL-1线性关系良好(r=0.999 1),杂质F在2.000~20.000 μg·mL-1线性关系良好(r=0.999 9); 3-氨基丙醇和杂质D的检测限分别为9.95、9.87 μg·mL-1,杂质F因色谱柱柱效降低且进样量过大未能进行检测限测定;3-氨基丙醇、杂质D、杂质F的定量限分别为19.90、19.74、2.000 μg·mL-1;起始物料、杂质D和杂质F回收率均在90.09%~115.90%,回收率RSD分别为4.8%、7.2%、2.3%。结论 该方法的专属性、精密度、线性关系良好,准确可靠,符合异环磷酰胺中3种有关物质的检测要求。 相似文献
6.
目的 建立枸橼酸坦度螺酮原料药中间体中潜在基因毒性杂质1,4-二溴丁烷的控制检测方法。方法 采用高效气相色谱(GC)法,使用色谱柱Agilent DB-624(30 m×320 μm,1.8 μm),升温程序:初始柱温95℃,保持2 min,以20℃/min升温至220℃,保持5 min。进样口温度250℃,检测器温度250℃,体积流量3 mL/min;分流比1∶1;进样量1 μL。进行专属性、线性范围、灵敏度、稳定性、重复性、回收率、耐用性方法学考察。结果 1,4-二溴丁烷在0.109 5~1.094 8 μg/mL内峰面积与质量浓度线性关系良好(r=0.998 6);检测限为0.109 5 μg/mL,定量限为0.273 7 μg/mL,平均回收率为116.2%,方法学考察均符合要求。各批次样品中1,4-二溴丁烷的质量分数均小于0.002 5%。结论 建立的方法专属性强、灵敏度高、测定结果准确、操作简单,可用于枸橼酸坦度螺酮原料药中间体中1,4-二溴丁烷的检测。 相似文献
7.
目的 建立测定阿戈美拉汀原料药中残留的2种有机溶剂(乙酸、乙醚)的检测方法。方法 采用直接进样气相色谱法,色谱柱为DB-FFAP毛细管柱(30 m×0.32 mm×0.5 μm),载气为高纯度氮气;柱温40℃,维持2 min,以50℃/min升至120℃;再以20℃/min升至220℃,维持2 min;氢火焰离子化检测器(FID),进样口温度为250℃,检测器温度为250℃,载气流量为2 mL/min,进样量1 μL,分流比为20∶1。结果 在考察的浓度范围内线性关系良好(r=0.999 7~0.999 8),2种残留溶剂均完全分离,精密度试验RSD值以及被测组分的平均回收率均符合要求。结论 该气相色谱法操作简单,准确度、灵敏度高,可用于检测阿戈美拉汀原料药中残留的有机溶剂。 相似文献
8.
目的 采用GC同时测定白芍总苷原料药中乙醇、乙酸乙酯和正丁醇3种残留溶剂。方法 检测器为氢火焰离子化检测器(FID),色谱柱为Agilent DB-624石英毛细管柱(30 m×0.53 mm,3.0 μm),溶剂为N,N-二甲基甲酰胺(DMF),程序升温。结果 3种残留溶剂均能完全分离,乙醇、乙酸乙酯和正丁醇分别在24.60~491.98 μg·mL-1(r=0.999 8),21.01~420.25 μg·mL-1(r=1.000 0),23.37~467.48 μg·mL-1(r=0.999 8)内与峰面积呈良好的线性关系,检测限分别为0.002 37%,0.000 08%和0.000 63%。结论 该方法简单可靠,灵敏度高,可用于白芍总苷原料中的残留溶剂控制。 相似文献
9.
目的 建立辅料乳糖的HPLC-RID检测方法。方法 色谱柱为Boston Green Amino氨基键合硅胶柱(250 mm×4.6 mm,5 μm),流动相为乙腈-水(70:30),体积流量1.0 mL/min,柱温45℃;检测器为示差折光检测器,检测器温度40℃,进样量10 μL。结果 乳糖在0.2~5.0 mg/mL范围内线性关系良好(r≥0.999 8),检测限为0.06 mg/mL,平均回收率为99.6%,相对标准偏差为0.7%。结论 该方法专属性好、操作简便、快速准确,适用于辅料乳糖的含量测定。 相似文献
10.
目的 建立UHPLC波长切换法同时测定芎菊上清丸中9种成分的含量方法。方法 采用Agilent Ecilipse C18(2.1 mm×100 mm,1.6 μm)色谱柱,流动相:甲醇-0.05%磷酸水溶液,梯度洗脱;流速为0.3 mL·min-1;检测波长:327,237,320,345,278,254 nm;柱温30℃;进样量2 μL;并采用SPSS 22.0统计软件对含量测定结果进行主成分分析与聚类分析。结果 绿原酸、3,5-二咖啡酰奎宁酸、栀子苷、甘草苷、阿魏酸、盐酸小檗碱、黄芩苷、升麻素苷、5-O-甲基维斯阿米醇苷线性范围分别为4.30~68.80 μg·mL-1(r=0.999 0)、6.66~106.56 μg·mL-1(r=0.999 2)、7.67~122.72 μg·mL-1(r=0.999 4)、4.88~78.08 μg·mL-1(r=0.999 1)、2.37~37.92 μg·mL-1(r=0.999 1)、6.50~103.92 μg·mL-1(r=0.999 2)、8.85~141.60 μg·mL-1(r=0.999 4)、0.88~14.08 μg·mL-1(r=0.999 7)、0.74~11.92 μg·mL-1(r=0.999 3);平均加样回收率(n=9)均在99.42%~103.10%,RSD均<2.0%。主成分分析与聚类分析均可将不同生产厂家的芎菊上清丸很好地分类,且分类结果一致。结论 所建立的多成分方法快捷、准确、重复性好,可用于芎菊上清丸的质量控制。 相似文献
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13.
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.相似文献
14.
Petrikovics I McGuinn WD Sylvester D Yuzapavik P Jiang J Way JL Papahadjopoulos D Hong K Yin R Cheng TC DeFrank JJ 《Drug delivery》2000,7(2):83-89
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. 相似文献
16.
《Critical reviews in toxicology》2013,43(5-6):327-369
AbstractThe 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. 相似文献
17.
Chang Min Kim Kun Ho Son Sung Hwan Kim Hyun Pyo Kim 《Archives of pharmacal research》1991,14(4):305-310
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. 相似文献
18.
Alberto García-Lled Javier Gmez-Pavn Juan Gonzlez del Castillo Teresa Hernndez-Sampelayo Mari Cruz Martín-Delgado Francisco Javier Martín Snchez Manuel Martínez-Sells Jos María Molero García Santiago Moreno Guilln Fernando Rodríguez-Artalejo Julin Ruiz-Galiana Rafael Cantn Pilar De Lucas Ramos Alejandra García-Botella Emilio Bouza 《Rev Esp Quimioter》2022,35(2):115
The precocity and efficacy of the vaccines developed so far against COVID-19 has been the most significant and saving advance against the pandemic. The development of vaccines has not prevented, during the whole period of the pandemic, the constant search for therapeutic medicines, both among existing drugs with different indications and in the development of new drugs. The Scientific Committee of the COVID-19 of the Illustrious College of Physicians of Madrid wanted to offer an early, simplified and critical approach to these new drugs, to new developments in immunotherapy and to what has been learned from the immune response modulators already known and which have proven effective against the virus, in order to help understand the current situation. 相似文献
19.
《Expert opinion on investigational drugs》2013,22(1):79-86
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. 相似文献