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1.
目的:建立HPLC法测定氯霉素注射液的有关物质(氯霉素二醇物和对硝基苯甲醛)和含量。方法:色谱柱采用ShiseidoC18 MGⅡ(250 mm×4.6 mm,5μm);流动相为甲醇-0.01 mol·L-1庚烷磺酸钠溶液(取磷酸二氢钾6.8 g,用0.01 mol·L-1庚烷磺酸钠溶液并稀释至1 000 ml,再加三乙胺5 ml,混匀,用磷酸调节pH至2.5)(32:68);流速为1.0 ml·min-1;检测波长为277 nm。结果:氯霉素、氯霉素二醇物、对硝基苯甲醛的线性范围分别为25.45~178.12μg·ml-1(r=0.999 8),7.95~63.60μg·ml-1(r=0.999 7)和1.86~7.44μg·ml-1(r=0.999 9)。氯霉素平均回收率为100.2%(RSD=0.6%)。结论:本文建立的高效液相色谱法结果准确可靠,专属性好,可作为氯霉素注射液有关物质和含量的测定方法。 相似文献
2.
目的:建立阿扎胞苷中多种有机溶剂残留量的测定方法。方法:采用项空气相色谱法,色谱柱为VF-624ms毛细管柱(60m×0.25mm,1.4μm),载气为氮气,氢火焰离子化检测器,柱温程序升温。结果:5种溶剂甲醇、异丙醇、二氯甲烷、甲酸甲酯、乙酸甲酯在此条件下能有效分离,且线性关系良好。甲醇,甲酸甲酯,异丙醇,乙酸甲酯,二氯甲烷的线性范围分别为10.32~127.89μg·ml-1(r=0.999 8),1.34~17.08μg·ml-1(r=0.999 9),3.44~43.16μg·ml-1(r=0.9999),1.47~16.94μg·ml-1(r=0.999 8),0.79~8.61μg·ml-1(r=0.999 4);平均回收率分别为97.7%(RSD=1.8%,n=6),100.0%(RSD=1.6%,n=6),99.3%(RSD=1.2%,n=6),101.2%(RSD=1.4%,n=6),99.7%(RSD=4.6%,n=6);检测限分别为5.16,0.67,1.72,0.74,0.40μg·ml-1。结论:该方法简单、准确、灵敏度高、重复性好,适合于阿扎胞苷中残留溶剂的检测。 相似文献
3.
目的:建立滴强灵胶囊中3组分的HPLC测定方法。方法:以COSMOSIL C18(250 mm×4.6 mm,5μm)为色谱柱,以醋酸铵溶液[0.25 mol·L-1醋酸铵溶液-0.05 mol·L-1EDTA-2Na溶液-三乙胺(100:10:1),用醋酸调pH至7.5]-乙腈(88:12)为流动相测定甲硝唑和土霉素的含量,流速1 ml·min-1,检测波长280 nn,柱温30℃;以甲醇-水(60:40)为流动相测定醋酸泼尼松的含量,流速1 ml·min-1,检测波长240 nm,柱温30℃。结果:建立的HPLC法能排除辅料对主药中3组分的干扰,甲硝唑、土霉素、醋酸泼尼松的含量测定的线性范围分别为0.04~0.80 mg·ml-1(r=0.999 9),0.02~0.40 mg·ml-1(r=0.999 9)和0.02~0.40 mg·ml-1(r=0.999 9);平均回收率分别为99.94%(RSD=0.07%)、99.85%(RSD=0.09%)、98.16(RSD=1.58%)(n=6)。结论:本法操作简便可靠,可用于滴强灵胶囊的质量控制。 相似文献
4.
目的:建立HPLC测定二维亚铁颗粒(Ⅱ)中维生素C和维生素B6含量的方法。方法:采用Insteril ODS-3色谱柱(250 mm×4.6 mm,5μm),流动相:0.03 mol·L-1磷酸氢二铵溶液(加入0.01%庚烷磺酸钠,用磷酸调节pH至3.0)-甲醇,梯度洗脱,检测波长为280 nm,流速:0.7~1.0 ml·min-1,柱温30℃。结果:维生素C与维生素B6分别在37~594μg·ml-1(r=0.999 9)与3~51μg·ml-1(r=1.000 0)范围内线性关系良好,平均回收率分别为99.6%与99.2%,RSD分别为0.48%与0.54%(n=9)。结论:本法简便、结果准确、可靠,可用于二维亚铁颗粒(Ⅱ)中维生素C、维生素B6的含量测定。 相似文献
5.
目的:建立高效液相色谱法同时测定肝复康丸中五味子醇甲、五味子酯甲、五味子甲素和五味子乙素等4种成分的含量测定方法。方法:采用Agilent TC-C18色谱柱(250 mm×4.6 mm,5μm);乙腈-水为流动相,梯度洗脱,流速0.8 ml·min-1;检测波长:254 nm。结果:五味子醇甲、五味子酯甲、五味子甲素、五味子乙素与其相邻杂质峰能完全分离,五味子醇甲、五味子酯甲、五味子甲素、五味子乙素的线性范围(相关系数)分别为68.62~686.25μg·ml-1(r=0.999 9),15.54~155.40μg·ml-1(r=0.999 8),6.45~64.50μg·ml-1(r=0.999 9)和15.57~155.70μg·ml-1(r=0.999 9)。平均回收率分别为100.80%,100.46%,101.06%和100.55%,RSD为1.31%,1.72%,2.00%和1.67%。结论:本方法简便、准确、重复性好,能排除其他成分的干扰,可用于该制剂的质量控制的评价。 相似文献
6.
目的:建立HPLC法同时测定口腔溃疡液中氯霉素、醋酸地塞米松及盐酸丁卡因等3组分的含量。方法:色谱柱采用Kromasil C18柱(250mm×4.6mm,5μm),甲醇-水-乙腈(45:45:10)(含0.02%庚烷磺酸钠,0.34%磷酸二氢钾,用三乙胺调pH至6.5)为流动相。检测波长240~340nm。结果:氯霉素在8.527-25.581mg·ml-1(r=0.9992),醋酸地塞米松在0.127~0.381mg·ml-1(r=0.999 9),盐酸丁卡因在5.014~15.019mg·ml-1(r=0.9992)浓度范围内线性关系良好。氯霉素的平均回收率为99.16%,RSD为0.47%;醋酸地塞米松的平均回收率为99.03%,RSD为0.62%;盐酸丁卡因的平均回收率为100.40%,RSD为1.16%。结论:该方法具有操作简便,结果准确的优点,可用于口腔溃疡液中的氯霉素、醋酸地塞米松及盐酸丁卡因的质量控制。 相似文献
7.
目的:建立降黏胶囊的质量标准。方法:用TLC法对水蛭和地龙进行定性鉴别;用HPLC法测定丹参素、大黄素、丹参酮ⅡA的含量。结果:薄层色谱图斑点清晰,阴性对照无干扰;丹参素钠、大黄素、丹参酮ⅡA分别在18.12~543.60μg·ml-1(r=0.999 6),4.86~145.92μg·ml-1(r=0.999 8),8.99~269.58μg·ml-1(r=0.999 4)范围内与峰面积呈良好线性关系,平均回收率分别为99.76%(RSD=0.71%,n=9),100.04%(RSD=1.48%,n=9),100.13%(RSD=1.16%,n=9)。结论:本方法简便、可靠、准确,可用于该制剂的质量控制。 相似文献
8.
目的:测定不同产地、品种的地龙药材中尿嘧啶、次黄嘌呤、尿苷、肌苷的含量,建立地龙质量控制的客观指标。方法:用0.9%生理盐水超声提取地龙药材,采用反相高效液相色谱法,Waters Symmetry C18色谱柱(150mm×4.6mm,5μm),以0.01mol·L-1磷酸二氢钾溶液和50%甲醇为流动相,流速为0.8ml·min-1,梯度洗脱,检测波长254nm,柱温27℃,同时测定尿嘧啶、次黄嘌呤、尿苷、肌苷等4种成分的含量。结果:尿嘧啶的线性范围为0.75~24.00μg·ml-1(r=0.9993),平均回收率99.82%,RSD=2.34%(n=6);次黄嘌呤的线性范围2.50~80.00μg·ml-1(r=0.9992),平均回收率101.93%,RSD=1.45%(n=6);尿苷的线性范围1.25~40.00μg·ml-1(r=0.9992),平均回收率97.53%,RSD=1.73%(n=6);肌苷的线性范围5.00~160.00μg·ml-1(r=0.9991),平均回收率102.06%,RSD=2.44%(n=6)。结论:该方法重复性,回收率好,可用于地龙药材中尿嘧啶等4种成分的含量测定。 相似文献
9.
目的:建立肠肽胶囊中三七有效成分的HPLC含量测定方法。方法:色谱柱为SinoChrom ODS-BP(150 mm×4.6mm,5μm),以乙腈(A)和水(B)为流动相,梯度洗脱,检测波长为203 nm,流速为1.0 ml·min-1,柱温为室温,进样量为20μl。结果:三七皂苷R1、人参皂苷Rg1及人参皂苷Rb1的线性范围依次为63.9~319.5μg·ml-1、112.6~563.2μg·ml-1、102.5~512.8μg·ml-1,线性关系良好(r值分别为0.999 7、0.999 4、0.999 9);三种皂苷的平均回收率分别为96.47%、98.75%,97.55%,RSD分别为1.52%、1.73%、1.81%(n=6)。结论:本方法简便可行、准确、灵敏度高、专属性强,可用于肠肽胶囊的质量控制。 相似文献
10.
目的:建立HPLC法同时测定跌打止痛贴膏中三七皂苷R1和人参皂苷Rg1含量的方法。方法:色谱柱为Shim-packCLC-ODS C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.05%磷酸溶液,梯度洗脱;检测波长203 nm,柱温35℃,流速1.0ml·min-1。结果:三七皂苷R1和人参皂苷Rg1线性范围分别为0.035 8~0.178 8 mg·ml-1(r=0.999 7),0.225 5~1.128 0mg·ml-1(r=0.999 6);平均回收率分别为96.8%(RSD=2.1%)和97.3%(RSD=2.2%)。结论:本方法简便可靠,重复性好,可用于测定跌打止痛贴膏中三七皂苷R1和人参皂苷Rg1的含量。 相似文献
12.
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.
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.
《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
19.
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