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目的:建立一种快速灵敏的同时测定十味龙胆花颗粒中的有效成分龙胆苦苷和小檗碱的HPLC—MS方法。方法:样品用50%甲醇溶液超声提取,采用Zorbax SBC18(4.6mm×250mm,5μm)色谱柱,以含0.2mmol·L^-1醋酸钠的1%醋酸水溶液(A)-甲醇(B)为流动相进行梯度洗脱(0~10min,33%B;19min,60%B;19.01min,80%B),流速0.8mL·min^-1;在ESI正离子模式下,采用选择性离子监测方法(0—14min,m/z 379;14~22min,m/z 336)。结果:龙胆苦苷、小檗碱的线性范围分别为0.030~30.0μg·mL^1(r=0.9992)和0.004~10.0μg·mL^-1(r=0.9990),检出限分别为0.010μg·mL^-1和0.0013μg·mL^-1样品加样回收率为99.2%~103.3%,日内、日间精密度试验的RSD均低于5%。结论:方法快捷、准确,重复性好,可用于药品十味龙胆花颗粒的分析。 相似文献
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目的用高效液相色谱法(HPLC法)测定利胆合剂中龙胆苦苷的含量。方法采用Shimpack C18色谱柱(150mm×6mm。5μm),流动相为甲醇-水(3:7),检测波长为258nm,流速为1.0mL/min。结果方法的平均加样回收率为95.6%,RSD=1.3%(n=5),龙胆苦苷进样量在0.125-1.0μg范围内与峰面积线性关系良好。结论方法准确、重现性好,可作为利胆合剂的含量测定方法。 相似文献
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HPLC法测定丹芩颗粒中黄芩苷和丹酚酸B的含量 总被引:2,自引:0,他引:2
目的:建立高效液相色谱法测定丹芩颗粒中黄芩苷和丹酚酸B的含量。方法:采用Dionex高效液相色谱仪,色谱柱为Diomand C18柱(200mm×4.6mm,5μm);测定黄芩苷的流动相为甲醇-水-磷酸(43:57:0.2),检测波长为280nm;测定丹酚酸B的流动相为甲醇-乙腈-水-甲酸(27:8:63:2),检测波长为286nm;流速为1.0mL·min^-1;柱温30℃。结果:在测定条件下,黄芩苷和丹酚酸B的浓度分别在15.0—90.2μg·mL^-1(r=0.9998)和48.7~207μg·mL^-1(r=0.9999)范围内线性关系良好;方法回收率(n=6)分别为98.3%(RSD=1.4%)和97.1%(RSD=1.2%)。结论:本方法操作简便,准确度高,专属性强,适用于丹芩颗粒的质量控制。 相似文献
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HPLC法测定小儿康颗粒中芍药苷的含量 总被引:1,自引:1,他引:1
建立HPLC法测定小儿康颗粒中芍药苷的含量。采用Phenomenex Luna C18色谱柱,以乙腈-0.1%磷酸(13:87)为流动相,流速:lmL·min^-1检测波长:230nm。芍药苷在21.48-107.4μg·mL。范围内线性关系良好,r=0.9996;加样回收率为100.0%。RSD=1.3%(n=6)。方法简便可行、准确,能有效控制小儿康颗粒质量。 相似文献
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RP—HPLC同时测定田基黄药材中异槲皮苷、槲皮苷和槲皮素的含量 总被引:1,自引:0,他引:1
目的:建立田基黄药材中异槲皮苷、槲皮苷和槲皮素的RP—HPLC同时含量测定方法。方法:使用Hypersil C18(250mm×4.6mm,5μm)柱,以乙腈(A)-0.02mol·L^-1磷酸二氢钾缓冲液(磷酸调pH3.0)(B)为流动相进行梯度洗脱(0~20min,A相为14%;20~35min,A相从14%变至30%;35~45min,A相从30%变至38%),流速:1.0mL·min^-1,检测波长:360nm,柱温:35℃。结果:异槲皮苷、槲皮苷和槲皮素浓度分别在9.90~330μg·mL^-1(r=0.9996,n=6)、19.2~640μg·mL^-1(r=0.9998,n=6)和2.16~72.0μg·mL^-1(r=0.9997,n=6)范围内与峰面积积分值线性关系良好;平均加样回收率(n=9)分别为97.2%,99.1%,98.9%。结论:不同购买地田基黄药材中异槲皮苷、槲皮苷和槲皮素含量存在较大差异;该方法简便可靠,重复性好,为田基黄药材质量控制提供了方法。 相似文献
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目的:建立测定芍连胃乐片中芍药苷和盐酸小檗碱含量的高效液相色谱法。方法:芍药苷含量测定采用C18(200mm×4.6mm,5μm),流动相为乙腈:0.05mol·L^-1磷酸二氢钾溶液(15:85),检测波长为230nm。盐酸小檗碱含量测定采用C18(250mm×4.6mm,5μm),流动相为乙腈:0.033mol·L^-1磷酸二氢钾溶液(32:68),检测波长为265nm。结果:芍药苷在3.0—48.3μg·ml^-1范围内线性关系良好(r=1.0000),平均回收率为98.1%,RSD为0.5%;盐酸小檗碱在1.0~16.4μg·ml^-1范围内线性关系良好(r=1.0000),平均回收率为98.9%,RSD为1.0%。结论:本方法简便、可靠、准确。 相似文献
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RP—HPLC法测定畅鼻通颗粒中升麻素苷和5-O-甲基维斯阿米醇苷的含量 总被引:1,自引:0,他引:1
目的:建立测定畅鼻通颗粒中升麻素苷和5-O-甲基维斯阿米醇苷含量的反相高效液相色谱法。方法:采用Agilent Eclipse XDB—C18柱(250mm×4.6mm,5μm),甲醇-水-三乙胺(35:65:0.1)为流动相,流速1.0mL·min^-1,检测波长254nm。结果:升麻素苷和5-O-甲基维斯阿米醇苷的线性范围分别为2.5~100.0mg·L^-1(r=0.9993)和2.1~84.0mg·L^-1(r=0.9992);平均回收率(n=9)分别为99.2%和99.8%。结论:该方法简单,结果准确、可靠,可以作为该制剂质量控制的一项重要指标。 相似文献
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高效液相色谱法测定茶黄酊中儿茶素、表儿茶素和黄芩苷的含量 总被引:2,自引:0,他引:2
目的:建立高效液相色谱法测定茶黄酊中儿茶素、表儿茶素和黄芩苷含量。方法:采用Agilent ZORBAX Eclipse XDB—C18(150mm×4.6mm,5μm)色谱柱;流动相A为0.5%三乙胺溶液(以磷酸调pH至3.0),流动相B为乙腈,梯度洗脱(0~12min,流动相B10%;12.1~30min,流动相B22%);流速:1mL·min^-1,检测波长278nm。结果:儿茶素、表儿茶素和黄芩苷线性范围分别为26.75—214.0μg·mL^-1(r=0.9998),5.568~44.54μg·mL^-1(r=0.9998),3.520~28.16μg·mL^-1(r=0.9999)。回收率(n=6)分别为99.8%,98.9%,102.6%;RSD分别为0.61%,1.2%,0.92%。结论:本方法简便、准确、稳定,重复性好,可用于茶黄酊中儿茶素、表儿茶素和黄芩苷的含量测定。 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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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
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《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
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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
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《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
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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