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1.
目的 建立HPLC法测定安立生坦中R异构体的方法。方法 采用HPLC法, 用硅胶键合蛋白质型手性色谱柱ULTRON ES-OVM(150 mm×4.6 mm, 5 μm);以0.02 mol/L磷酸二氢钾溶液(用磷酸调节pH至4.0)-乙腈(80:20)为流动相;检测波长220 nm;柱温30 ℃;体积流量为1.0 mL/min;进样体积20 μL。结果 安立生坦R异构体在0.501~4.008 μg/mL与峰面积线性关系良好(r=0.999 3), 平均回收率为98.62%, RSD值为2.82%(n=12)。结论 本法操作简便快速, 结果准确可靠, 可用于安立生坦中R异构体的控制。 相似文献
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目的 建立测定注射用头孢唑肟钠中有关物质的HPLC法。方法 采用Agient Eclipse C18色谱柱(250 mm×4.6 mm,5 μm);以乙腈–pH 3.6缓冲液(取枸橼酸1.42 g、磷酸氢二钠2.31 g,加水溶解并稀释至1 000 mL)为流动相,进行梯度洗脱;检测波长:254 nm;柱温:40℃;体积流量:0.8 mL/min;进样量20 μL。结果 头孢唑肟在0.24~14.52 μg/mL与峰面积呈良好的线性关系(r=1.000 0),最低检出质量浓度0.03 μg/mL。结论 采用的HPLC方法简单、专属性强,可有效控制注射用头孢唑肟钠产品的质量。 相似文献
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目的 建立测定富马酸喹硫平缓释片含量及4种有关物质的HPLC方法。方法 采用ZorBAX Eclipse XDB-C8柱(4.6 mm×250 mm,5 μm),以甲醇-乙腈-0.02 mol/L磷酸氢二铵溶液(54:7:39)为流动相,体积流量为1.0 mL/min;柱温为30℃;检测波长为230 nm。结果 在该色谱条件下,有关物质与主成分分离度良好,R均大于1.5;富马酸喹硫平在80~320 μg/mL线性良好,r=0.999 7,检测限为0.025 μg/mL;平均回收率为99.9%(RSD=1.7%,n=9)。结论 该方法简便、灵敏、重复性好,可用于同时测定富马酸喹硫平缓释片的含量及4种有关物质。 相似文献
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目的 运用高效液相色谱法对苍耳子中的绿原酸及辛夷中的木兰脂素进行含量测定。方法 绿原酸采用高效液相色谱法,色谱柱为Shim-Pack CLC ODS C18柱(250×4.6 mm,5 μm);乙腈-0.4%磷酸溶液(10∶90)为流动相;检测波长为327 nm;流速:1.0 mL/min。木兰脂素的色谱条件为:用辛基键合硅胶为填充剂Hypersil C8柱(250×4.6 mm,5 μm)为色谱柱;乙腈-四氢呋喃-水(35∶1∶64)为流动相;检测波长为278 nm;流速:1.0 mL/min。结果 绿原酸在12.99~129.90 μg/mL(r=0.999 9)范围内及木兰脂素在19.67~196.70 μg/mL(r=0.999 9)范围内线性关系良好,绿原酸回收率为99.28%,RSD为1.15%(n=9);木兰脂素回收率为99.42%,RSD为0.68%(n=9), 3批样品中绿原酸的平均含量为0.818 4、0.818 5、0.818 9 mg/mL;木兰脂素的平均含量为0.163 7、0.163 4、0.164 1 mg/mL。结论 高效液相色谱法简便、灵敏、准确,可作为苍辛滴鼻剂的定量质量控制。 相似文献
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目的 建立高效液相色谱法测定乙酰谷酰胺中异构体N-乙酰-D-谷氨酰胺的含量测定方法。方法 采用高效液相色谱法,直链淀粉-三(S)-α-甲苯基氨基甲酸酯为填充剂(AS-H 4.6 mm×250 mm,5 μm)手性色谱柱;检测波长210 nm,柱温30 ℃,流动相为正己烷(每1 000 mL加0.5 mL三氟乙酸和0.5 mL三乙胺):无水乙醇(每1 000 mL中加0.5 mL三氟乙酸和0.5 mL三乙胺)=90:10。结果 浓度在1.289 3~36.099 5 μg·ml-1范围内线性关系良好(r=0.998 2,n=5),平均回收率94.9%,RSD=1.6%(n=9),方法的检测限LOD为0.314 6 μg·ml-1,定量限1.258 4 μg·mL-1。结论 所用方法专属性强、结果准确、稳定性好,适用于乙酰谷酰胺中异构体N-乙酰-D-谷氨酰胺的检测。 相似文献
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目的 建立格列喹酮片体外溶出度HPLC检测方法及溶出曲线评价。方法 色谱柱为Diamonsil@Plus C18(150 mm×4.6 mm,5 μm);流动相为磷酸二氢铵溶液(取磷酸二氢铵1.725 g,加水300 mL溶解后,用磷酸调节pH值至3.5±0.1)-乙腈(3:5);体积流量1.0 mL/min;检测波长为310 nm,进样量20 μL,柱温为35℃,外标法计算。结果 空白辅料、溶出介质不干扰测定;格列喹酮在3.13~50.02 μg/mL线性关系良好(r=0.999 8,n=7);格列喹酮平均回收率为100.2%(RSD=0.83%,n=9);格列喹酮溶出度溶液在0~24 h内稳定性良好(RSD=0.51%,n=7);弃去10 mL初滤液后滤膜吸附达到饱和。自研品和参比制剂在7种不同pH溶出介质中溶出行为一致。结论 经方法学考察,反相高效液相色谱法测定格列喹酮片溶出度专属性强,准确可靠,易于操作。 相似文献
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目的 建立测定肌瘤化消颗粒中淫羊藿苷和丹参酮IIA的HPLC法。方法 采用高效液相色谱法,DiamonsilTM C18色谱柱(250 mm×4.6 mm,5 μm);流动相:乙腈-水,梯度洗脱;检测波长为270 nm;柱温为40℃;体积流量为1.0 mL/min;进样量10 μL。结果 淫羊藿苷在7.5~50 μg、丹参酮IIA在3~20 μg与峰面积的线性良好(r=0.999 9)。平均回收率分别为100.2%、100.1%,RSD值分别为0.9%、1.3%(n=9)。结论 本法操作简便,重现性好,可有效控制肌瘤化消颗粒的质量。 相似文献
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HPLC测定他达拉非中的对映异构体和非对映异构体 总被引:1,自引:1,他引:0
目的 建立他达拉非原料药中对映异构体和非对映异构体的定量分析方法。方法 采用CHIRALPAK-IC(250 mm×4.6 mm,5 μm)色谱柱,流动相为乙腈-水(40:60),流速为1.0 mL·min-1,检测波长为222 nm,柱温为30℃,进样量20 μL。加校正因子的自身稀释对照法计算异构体含量,其中异构体A、异构体B和异构体C的校正因子分别为1.22,1.07和1.25。结果 他达拉非及异构体A、异构体B和异构体C峰分离良好,分离度>1.5,异构体A、异构体B和异构体C分别在25.3~379.5,50.6~379.5,50.4~378.0 ng·mL-1内线性关系良好(r为0.997 3~0.998 7),加样回收率分别为107.5%,96.9%,98.5%(n=9),进样精密度RSD≤2%,重复性RSD分别为1.44%,1.64%和4.89%。检测限分别为12.7,25.3,25.2 ng·mL-1。3批样品中异构体A最高含量为0.018%,异构体B及异构体C均未超过检测限(<0.010%)。结论 该方法简单,准确,重复性好,可用于他达拉非原料药中对映异构体和非对映异构体的测定。 相似文献
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目的 建立高效液相色谱(HPLC)法测定瑞舒伐他汀钙原料药中有关物质的方法。方法 采用HPLC法,Phenomenex Luna C18 (2)色谱柱(250 mm×4.6 mm,5 μm),流动相为水-乙腈-1%三氟乙酸水溶液(62:37:1),体积流量为1.0 mL/min,柱温为40℃,进样量为20 μL,检测波长为242 nm。结果 系统和方法精密度RSD值均小于20%(n=6),瑞舒伐他汀钙在0.020 1~0.201 3 μg线性关系良好(r=0.999 8),瑞舒伐他汀钙的检测限为2.76 ng,各杂质氧化产物、内酯、光降解产物Ⅰ和Ⅱ和非对映异构体各杂质的检测限依次为1.85、1.32、1.08、1.11、2.06 ng。结论 本法合理严谨,精密度好,检测灵敏度高,可有效用于瑞舒伐他汀钙有关物质检测。 相似文献
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目的 建立衍生化法分离(2R,4R)-4-甲基-2-哌啶甲酸乙酯酒石酸盐(MPFET)3种手性异构体。方法 以2,3,4,6-四-O-乙酰基-β-D-吡喃葡萄糖异硫氰酸酯(GITC)为柱前衍生化试剂,对MPFET手性异构体进行分离,并对衍生化条件进行优化。采用Venusil AQ C18(250 mm×4.6 mm,5 μm)色谱柱作为固定相进行分离、监测和定量。以0.01 mol/L磷酸二氢钾溶液(用磷酸调pH至3.6)-乙腈(60∶40)为流动相,体积流量1.5 mL/min进行等度洗脱,采用紫外检测器,检测波长266 nm;柱温30℃;进样量20 μL。结果 MPFET与2S,4S-异构体分离度为1.76。2S,4R-异构体的线性范围为1.500~8.999 μg/mL,2R,4S-异构体的线性范围为0.255 2~1.531 0 μg/mL,2S,4S-异构体的线性范围为0.250 1~75.000 0 μg/mL,MPFET的线性范围为0.250 1~600.100 0 μg/mL,回收率均在90%~108%内,RSD均不大于3.0%。结论 柱前衍生化法分离MPFET中3种手性异构体,专属性强、准确度高、灵敏度高、重复性好,可用于MPFET手性异构体的分离和质量控制。 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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