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1.
高效液相色谱法测定灯盏花素注射液含量 总被引:1,自引:0,他引:1
目的 :建立高效液相色谱法测定灯盏花素注射液含量的方法。方法 :色谱柱 μ- Bondapak C1 8钢柱 ( 4 .6 mm×2 0 0 mm,10μm) ,流动相为甲醇 -水 ( 6 0∶ 4 0 ) ,流速为 0 .6 ml/ min,检测波长 335 nm。结果 :灯盏花素注射液在 10 .0~ 5 0 .0mg/ L浓度范围内 ,线性关系良好 ,r=0 .9996 ,平均加样回收率为 10 0 .31% ,RSD为 1.19% ( n =6 )。结论 :本法简便 ,结果准确 ,可用于灯盏花素注射液的质量控制 相似文献
2.
HPLC测定灯盏花素缓释胶囊含量 总被引:1,自引:1,他引:1
目的建立灯盏花素缓释胶囊中野黄芩苷的高效液相色谱法(HPLC)含量测定方法。方法采用高效液相色谱法,C18柱色谱柱(4.6mm×x150mm,5μm),柱温30℃;进样量10μL,流动相:甲醇-四氢呋喃-0.1%磷酸溶液(14:14:72),流速1.0mL-min^-1;检测波长335nm。结果野黄芩苷在24.45~293.46μg·mL^-1范围内,峰面积与浓度的线性关系良好(r=0.9999),野黄芩苷平均回收率为101.5%,RSD为3.616%。结论该方法简便准确,重现性好,可用于灯盏花素缓释胶囊的质量控制. 相似文献
3.
目的:建立运用HPLC法同时测定葛根芩连汤中8种有效成分(葛根素、甘草苷、黄芩苷、汉黄芩苷、巴马汀、小檗碱、黄芩素、汉黄芩素)的含量。方法:采用反相高效液相色谱法测定,色谱柱:Agilent ZORBAX Eclipse SB-C18(4.6 mm×250 mm,5μm);流动相:甲酸铵(pH3.0、10 mmol.L-1)-乙腈,梯度洗脱;流速:1 mL.min-1;检测波长:270、360 nm;柱温:25℃;进样量:20μL。结果:葛根素、甘草苷、黄芩苷、汉黄芩苷、巴马汀、小檗碱、黄芩素、汉黄芩素的质量浓度分别在1.12~22.3μg.mL-1(r=0.9990),1.08~21.7μg.mL-1(r=0.9991),4.10~82.0μg.mL-1(r0.9990),1.23~24.6μg.mL-1(r=0.9993),1.99~39.8μg.mL-1(r=0.9991),4.05~81.0μg.mL-1(r=0.9993),2.40~48.0μg.mL-1(r=0.9994),1.11~22.1μg.mL-1(r=0.9993)范围内与色谱峰面积呈良好的线性关系。平均回收率(n=5)均在95%~10... 相似文献
4.
目的建立β-葡萄糖醛酸苷酶解法与LC-MS-MS法相结合测定人体血浆中灯盏乙素的苷元,研究健康男性单剂量口服灯盏花素分散片的药代动力学。方法血浆样品经β-葡萄糖醛酸苷酶水解,甲醇蛋白沉淀,色谱柱为Agilent ZORBAX SB C18(2.1 mm×150 mm,5μm),运用乙腈-甲醇-水洗脱,多反应监测(MRM)灯盏乙素苷元([M-H]-,m/z285.0/136.8)和内标槲皮素([M-H]-,m/z 301.1/120.8)。12名健康男性单剂量口服灯盏花素分散片120 mg后,采用该方法测定血浆中灯盏乙素苷元,使用DAS 1.0软件处理数据,计算药代动力学参数。结果灯盏乙素苷元在4.01~513.38μg·L-1范围内线性良好,日内日间精密度小于7.22%,提取回收率大于84.23%。12名健康男性单剂量口服灯盏花素分散片120 mg后,以灯盏乙素苷元为检测对象的主要药动学参数为:Cmax(μg·L-1):159.97±58.14;AUC(0-19)(μg·L-1·h):1151.37±279.80;AUC(0-∞)(μg·L-1·h):1194.13±264.51;Tmax(h):6.33±1.67;T1/2(h):2.83±0.60。结论建立的酶解与LC-MS-MS相结合分析方法准确灵敏,适用于灯盏乙素人体内的药代动力学研究。 相似文献
5.
目的:建立仔花感冒胶囊中黄芩苷含量测定的HPLC方法。方法:用Kromasil-C_(18)柱(250mm×4.6mm,5μm),甲醇- 0.4%磷酸(54:46)为流动相,流速1.0m1.min~(-1),检测波长为315nm。结果:黄芩苷在0.11~0.64μg(r=0.999 9)范围内呈良好的线性关系,平均回收率为100.2%(RSD=1.4%,n=6)。结论:方法准确可靠,重复性好,可用于仔花感冒胶囊的质量控制。 相似文献
6.
目的:建立测定人血浆中灯盏乙素浓度的HPLC-MS/MS法。方法:采用Platisil ODS色谱柱(250 mm×4.6 mm,5μm),流动相为0.3%甲酸水溶液-甲醇(40∶60),流速为1.0 mL.min-1,以黄芩苷为内标,经乙酸乙酯萃取后,采用电喷雾电离化(ESI)方式和多反应离子监测(MRM)模式进行负离子检测,用于定量分析离子反应分别为m/z 461.1→285.1(灯盏乙素)和m/z 445.1→269.1(黄芩苷)。结果:线性检测范围为0.20~50.00μg.L-1,最低定量浓度0.20μg.L-1,r=0.999 3。低、中、高3个浓度的提取回收率分别为63.5%,69.5%,66.8%,基质效应分别为105.7%,97.5%,96.5%。结论:本法样品处理简单、快速,专属性强,灵敏度高,可用于灯盏乙素在人体内的药代动力学研究。 相似文献
7.
目的建立灯盏花素分散片的质量标准。方法采用薄层色谱法对灯盏花素分散片中野黄芩苷进行定性鉴别,建立灯盏花素分散片中焦袂康酸的限量检查方法,并采用高效液相色谱法对野黄芩苷进行含量测定。结果薄层色谱斑点清晰,专属性好;焦袂康酸对照品进样量在0.010 2~0.848μg范围内与峰面积线性关系良好(r=0.999 0),平均加样回收率为98.74%,RSD为0.92%(n=6);野黄芩苷对照品进样量在0.053~2.12μg范围内与峰面积线性关系良好(r=0.999 8),平均加样回收率为99.01%,RSD为1.11%(n=6)。结论所建立的方法准确简便、专属性强、重现性好,可以有效控制灯盏花素分散片的质量。 相似文献
8.
变换波长HPLC法同时测定藿香鼻炎合剂中五种成分的含量 总被引:1,自引:0,他引:1
目的建立HPLC波长切换联合梯度洗脱法同时测定藿香鼻炎合剂中的广藿香酮、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素含量的方法。方法采用Kromasil C_(18)(4.6 mm×250 mm,5μm)色谱柱;流动相A:乙腈,流动相B:0.4%磷酸溶液,进行梯度洗脱;流速:1.0 mL/min;柱温:30℃;检测波长分别规定为310 nm(广藿香酮)、280 nm(黄芩苷、汉黄芩苷、黄芩素和汉黄芩素)。结果广藿香酮、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素的线性范围分别为4.300~86.00μg/mL(r=0.999 6)、15.87~317.4μg/mL(r=0.999 8)、6.920~138.4μg/mL(r=0.9999)、6.340~126.8μg/mL(r=0.999 4)、5.250~105.0μg/mL(r=0.999 8),平均加样回收率和RSD均符合中国药典规定。结论本文建立的HPLC波长切换联合梯度洗脱法同时测定广藿香酮、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素5个成分,方法专属性强,重复性好,可作为藿香鼻炎合剂全面可靠的质量控制方法。 相似文献
9.
HPLC测定黄芩中6个成分的含量 总被引:5,自引:2,他引:3
目的建立高效液相色谱法对黄芩中6个成分(黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、白杨素、千层纸素A)的含量分析方法。方法采用Agilent ZORBAX SB-C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-0.3%磷酸三乙胺(B)为流动相,梯度洗脱,检测波长为275 nm,流速1.0 mL.min-1,柱温30℃。结果黄芩中的6个成分黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、白杨素、千层纸素A进样量分别在0.416 7~4.167μg(r=0.999 2)、0.078 15~0.781 5μg(r=0.999 5)、0.053 21~0.532 1μg(r=0.999 3)、0.016 36~0.163 6μg(r=0.999 3)、0.001 160~0.011 60μg(r=0.999 1)、0.010 46~0.104 6μg(r=0.999 4)范围内呈良好线性关系;平均回收率(n=5)分别为99.4%、100.1%、99.9%、100.2%、100.4%、100.1%,RSD分别为1.9%、2.2%、2.3%、1.6%、2.2%、2.1%。结论该方法准确可靠、重复性好,为黄芩质量综合评价提供了科学依据。 相似文献
10.
HPLC法同时测定黄芩中黄芩苷、黄芩素、汉黄芩素的含量 总被引:2,自引:0,他引:2
目的:建立反相高效液相色谱法同时测定黄芩中黄芩苷、黄芩素、汉黄芩素的含量.方法:采用Agilent Eclipse XDB-C18(250 mm×4.6 mm,5μm)色谱柱,以甲醇-乙腈-0.1%磷酸溶液为流动相,梯度洗脱;检测波长为277 nm;流速1.0 ml·min -1;进样量10 μl;柱温35℃.结果:黄芩苷、黄芩素、汉黄芩素的线性范围分别为0.059 ~ 1.175 μg,r=1.000 0(n =7)、0.010~0.204μg,r=1.000 0(n =7)和8.210×10-3~1.642×10-1 μg,r =1.000 0(n =7);提取回收率分别为99.08%,RSD=0.5%(n=6)、98.66%,RSD =0.5% (n =6)和98.31%,RSD =0.7% (n =6).结论:本法操作简便、快速、结果准确,可用于黄芩的质量控制. 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