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1.
目的:采用Q-TRAP LC-MS/MS测定中药白及中活性成分militarine、原儿茶酸和咖啡酸的含量。方法:采用Supelco Discovery C-18(150 mm×2.1 mm,3μm)色谱柱,以乙腈和水(含体积比0.1%甲酸)为流动相,梯度洗脱,流速为0.25 ml·min-1,AB Sciex 4000 Q-TRAP型质谱仪多重反应监测(MRM)扫描模式对白及对照药材和白及样品分别进行检测。结果:白及对照药材中militarine、原儿茶酸和咖啡酸的含量分别为1.167 5,0.062 6,0.001 0 mg·g-1.白及供试品药材中militarine、原儿茶酸和咖啡酸的含量分别为0.708 8,0.001 1,0.000 4 mg·g-1(n=3)。结论:该方法简便、准确、重现性好,可用于对中药白及中militarine、原儿茶酸和咖啡酸这三个成分进行定量分析。  相似文献   

2.
目的建立高效液相色谱法(HPLC法)测定胃康灵胶囊中甘草次酸含量的方法,以便于控制其质量。方法D IKMA C18柱(200mm×4.6mm,5μm),流动相为甲醇-水-冰醋酸(85∶14.5∶0.5),流速为1m l.m in-1,检测波长为250nm,柱温为20℃,在15m in内检测完毕。结果甘草次酸在0.996~2.998μg范围内与峰面积呈良好线性关系,r=9999,平均加样回收率为99.90%,RSD=1.30%(n=5)。结论首次用高效液相色谱法测定胃康灵胶囊中甘草次酸的含量,本法简便、快速、准确,可以用于胃康灵胶囊的质量控制。  相似文献   

3.
高效液相色谱法测定胃康灵胶囊中芍药苷的含量   总被引:3,自引:2,他引:3  
目的:建立高效液相色谱法(HPLC法)测定胃康灵胶囊中芍药苷含量的方法.方法:色谱柱为KramasiL C18柱(250 mm×4.6 mm,5μm),以乙腈-0.1%磷酸溶液(15:85)为流动相,流速为0.8 mL/min,检测波长为230 nm,柱温为30℃.结果:芍药苷进样量在0.31~0.92 μg范围内与峰面积线性关系良好(r=1.000),方法的平均回收率为99.5%,RSD为2.35%.结论:高效液相色谱法简便、准确,重现性好,可作为胃康灵胶囊的含量测定方法.  相似文献   

4.
[摘 要]目的:建立胃康灵胶囊中金胺O染色物的检测方法,并对其进行筛查,同时建立阳性样品中金胺O的含量测定方法。方法:采用UPLC-PDA法对胃康灵胶囊中的金胺O进行筛查,并采用UPLC-MS/MS二级质谱对阳性样品进行确证。结果:对来自37家企业的123批次样品进行筛查和确认发现:有6家企业的23批次样品中检出金胺O;金胺O进样在0.42~208.72 ng 的范围内有良好的线性关系。胃康灵胶囊阳性样品中金胺O的含量在1.0~28.7μg?粒-1。结论:本方法准确可靠,可作为胃康灵胶囊中金胺O染色物的检测方法。  相似文献   

5.
白及药材HPLC指纹图谱研究   总被引:2,自引:0,他引:2       下载免费PDF全文
郑江萍  雷震  黄良永 《中国药师》2013,(11):1611-1614
目的:建立白及药材化学成分的HPLC指纹图谱,为白及药材的质量控制提供科学依据。方法:采用HPLC法,以Waters SunFire C_(18)(250 mm×4.6 mm,5μm)为色谱柱,Diamonsil C_(18)保护柱,以乙腈和水为流动相,梯度洗脱,流速为1.0 ml·min~(-1),检测波长为270 nm,柱温为30℃。结果:15批白及药材化学成分特征图谱共检出9个分离度良好的共有峰。白及药材9个特征峰进行聚类分析,白及药材产地与特征图谱相似度差异不大。样品中参照物1,4-二[4-(葡萄糖氧)苄基]-2-异丁基苹果酸酯(militarine)的含量有明显差别。结论:该法简便、快速,可作为白及的质量控制的有力手段。  相似文献   

6.
目的: 建立白及中2-异丁基苹果酸葡萄糖氧基苄酯类成分的UPLC-ESI-Q/TOF-MS快速识别鉴定方法,以及主成分militarine的UPLC测定方法。方法: 液质联用方法采用Waters Acquity UPLC BEH C18(1.7 μm,2.1 mm×100 mm)色谱柱,乙腈-0.1%甲酸溶液梯度洗脱,检测器为高分辨四极杆飞行时间质谱,ESI离子源,MSEE代表碰撞能量)采集方式,采集质量数范围m/z 100~1 000。含量测定采用UPLC法,以乙腈-0.1%磷酸溶液(22:78)为流动相;检测波长为223 nm;柱温:35℃;流速:0.2 mL·min-1结果: 利用建立的白及化学成分数据库,结合2-异丁基苹果酸葡萄糖氧基苄酯类成分的诊断离子、准确分子量、质谱碎片及对照品信息,快速分析鉴定21个目标化合物。主成分militarine在19.059 0~381.180 8 μg·mL-1范围内线性关系良好(r=0.998 6)。加样回收率为100.9%,RSD为1.5%。36批白及中militarine的含量范围是1.5%~4.6%。结论: UPLC-Q/TOF-MS法能快速、准确地鉴定白及中的化学成分,为其药效物质基础研究提供科学依据。建立的UPLC含量测定方法操作简便、准确可靠,可用于白及的质量控制。  相似文献   

7.
目的:建立胃康灵胶囊中甘草次酸含量测定的方法。方法高效液相色谱法,Luna(月神)C18分析柱(250×4.6mm,5μ),甲醇-水(磷酸调PH 3.3)(90:10)(v/v)为流动相,流速1 mL/min,检测波长为250nm。结果甘草次酸在27-135μg/mL范围内线性关系良好(r=0.9994),方法的平均回收率为98.11%,RSD为0.81%。结论方法简便、准确、快速,可作为该制剂中甘草次酸的含量测定的方法。  相似文献   

8.
曾赣惠  苏长安 《江西医药》2011,46(12):1133-1135
目的建立胃康灵胶囊中芍药苷的含量测定方法。方法采用高效液相色谱法测定,Diamonsil C18色谱柱,以乙腈-0.1%磷酸溶液(14:88)为流动相,流速为1.0ml/min,柱温为30℃,检测波长为230nm。结果芍药苷在6.68-167.0μg/ml范围内具有良好的线性关系(r=0.9999),平均回收率为99.0%,RSD为0.84%。结论该方法简便、稳定、准确、重复性好,可用于胃康灵胶囊的质量控制。  相似文献   

9.
曾赣惠  苏长安 《江西医药》2011,46(11):1044-1045
目的建立胃康灵胶囊的薄层色谱鉴别方法。方法采用薄层色谱法鉴别胃康灵胶囊中的甘草、白及、延胡索及三七。结果利用薄层色谱法能检测出胃康灵胶囊中的甘草、白及、延胡索及一三七,薄层色谱图中斑点清晰,阴性对照无十扰。结论该方法简便、专属性强,可用于胃康灵胶囊的质量控制。  相似文献   

10.
刘冰冰  朱克旭 《安徽医药》2008,12(8):693-694
目的建立他克莫司胶囊含量的测定方法。方法采用高效液相色谱法,色谱柱为Kromasil 100-5C18柱(250mm×4.6mm,5μm),流动相为流动相:乙腈-水-磷酸(700:300:1),柱温为60℃,流速1.0ml·min^-1,检测波长为215nm;对3批他克莫司胶囊进行含量测定。结果他克莫司浓度在12.5~125mg·L^-1范围内,峰面积和浓度线性关系良好,平均回收率为98.8%(n=9),RSD=1.20%;3批样品中他克莫司含量分别为98.81%,98.67%,98.92%。结论该法测定他克莫司胶囊的含量,简便快捷,结果准确,重现性好,易于操作,可用于他克莫司胶囊含量的测定。  相似文献   

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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   

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14.
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   

15.
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   

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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.  相似文献   

18.
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   

19.
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   

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