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1.
目的 建立同时测定格拉司琼-舒芬太尼及格拉司琼-曲马多-芬太尼含量的方法.方法 采用HPLC法,分析柱为Agilent hypersil C18柱(125 mm×4.0 nm,5μm),流动相为0.02 mol·L~(-1)磷酸二氢钾(加0.6%三乙胺,磷酸调pH4.0)-乙腈,梯度洗脱,流速为1 mL·min~(-1),检测波长为220 nm.结果 格拉司琼、舒芬太尼、曲马多、芬太尼的线性范围分别为5~50μg·mL~(-1)(r=0.9999)、0.25~4.00 μg·mL~(-1)(r=0.9994)、20~70 μg·mL~(-1)(r=0.9996)、2.5~20.0μg·mL~(-1)(r=0.9999);其平均回收率分别为99.97%、98.75%、99.80%、100.53%.结论 所建方法可同时测定格拉司琼-舒芬太尼及格拉司琼-曲马多-芬太尼混合溶液的含量,且简便、准确、灵敏. 相似文献
2.
目的:建立测定人血清中舒芬太尼浓度的简便方法。方法:血清中舒芬太尼用乙酸乙酯-石油醚(4:1)单步提取后采用反相高效液相色谱法进行测定,其中色谱柱为Symmetry C18,流动相为乙腈-0.02mol.L-1醋酸铵-盐酸(pH4.3)(45:55),检测波长为230nm,柱温为室温,内标为艾司唑仑。结果:舒芬太尼血药浓度在0.025~4.000μg.mL-1范围内线性关系良好(r=0.9999);日内、日间RSD分别为3.49%~4.51%、4.67%~5.99%,平均回收率为101.92%~107.04%。结论:本方法提取步骤少,方法简单、快速、专一性强、准确,适合人血清中舒芬太尼的浓度监测。 相似文献
3.
QI Si-hua HE Zhen-qiu SUN Bo HUANG Li-jun 《药物分析杂志》2008,28(4):599-601
目的:建立测定人血浆中舒芬太尼血药浓度的 HPLC 方法。方法:以丁丙诺啡为内标,采用正己烷-无水乙醇(19:1,v/v)进行液-液萃取。采用 Diamonsil—C_(18)柱(4.6 mm×200mm,5μm),以0.01 mol·L~(-1)KH_2PO_4-乙腈(65:35,v/v,pH 5.6)为流动相,流速为1.5 mL·min~(-1),检测波长230 nm。结果:舒芬太尼在7.8125~12500 ng·mL~(-1)范围内线性关系良好(r=0.9976),最低检测浓度为4 ng·mL~(-1)。高、中、低浓度(12500,625,31.25 ng·mL~(-1))样本方法的平均回收率均大于97%;高、中、低浓度(12500,625,31.25 ng·mL~(-1))样本日内变异分别为4.65%,6.72%,6.68%,日间变异分别为8.65%,7.49%,13.19%。结论:本方法简便,准确,稳定性好,能够满足血浆中低浓度舒芬太尼的测定及临床药代动力学研究的要求。 相似文献
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目的建立早孕妇女血和胚胎组织中氟康唑浓度测定的RP-HPLC法。方法血和胚胎组织样品采用1 mol·L~(-1) NaOH溶液碱化、乙酸乙酯萃取后行HPLC测定。色谱柱:Diamonsil~(TM)C_(18)(200 mm×4.6 mm,5μm),流动相:乙腈-0.03 mol·L~(-1)磷酸盐缓冲液(pH 5.8,25:75,V/V),流速1.2 mL·min~(-1);检测波长260 nm;柱温40℃。结果血、胚胎组织样品分别在0.2~10 mg·L~(-1)和0.133~6.667μg·g~(-1)浓度范围内线性良好,最低检测浓度分别为0.1 mg·L~(-1)和0.066 7μg·g~(-1),方法回收率为96.56~104.35%,日内RSD≤6.81%,日间RSD≤4.78%,血和胚胎组织中氟康唑的萃取回收率均>70%。结论此法能简便、灵敏、准确地测定早孕妇女血和胚胎组织中氟康唑的浓度,可用于临床药动学研究。 相似文献
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《沈阳药科大学学报》2019,(4):327-333
目的建立一种毛细管气相色谱法,同时测定原料药奥希替尼中5种残留溶剂乙醇、乙腈、乙酸乙酯、二氯甲烷、1,4-二氧六环的含量。方法以Thermo TG-5MS毛细管柱(30 m×0.32 mm,0.25μm)为色谱柱,以氮气为载气,程序升温:起始柱温为30℃,保持10 min,之后以15℃·min~(-1)的速率升至150℃,保持4 min。采用直接进样法,进样体积为1μL。结果 5种有机溶剂在建立的色谱条件下分离度较高,且在质量浓度10.00~200.00 mg·L~(-1)内线性关系良好(r≥0.999 5),乙醇、乙腈、乙酸乙酯、二氯甲烷和1,4-二氧六环的检测限质量浓度分别为0.68、1.23、2.81、1.81和2.93μg·mL~(-1),定量限质量浓度分别为1.68、3.76、9.48、3.38和9.54 mg·L~(-1),平均回收率分别为100.4%、101.2%、102.7%、103.0%、101.2%,RSD分别为2.31%、3.53%、3.61%、4.71%、2.47%。利用该方法对3批奥希替尼样品中的残留溶剂进行检查,结果显示,乙醇的残留量分别为0.059%、0.064%和0.060%,乙酸乙酯的残留量分别为0.263%、0.260%、0.267%,乙腈、二氯甲烷和1,4-二氧六环未被检测出。结论该色谱方法可用于测定原料药奥希替尼中5种有机溶剂的含量。 相似文献
6.
《沈阳药科大学学报》2018,(2):98-102
目的建立HPLC法测定左卡尼汀中有关物质。方法采用Thermo APS-2 HYPERSIL色谱柱(250 mm×4.6 mm,5μm),流动相为磷酸盐缓冲液(含磷酸二氢钾质量浓度为6.81 g·L~(-1),用氢氧化钠试液调节pH值至4.7)-乙腈(体积比为35∶65);检测波长为205 nm;柱温为30℃;流速为1m L·min~(-1)。结果左卡尼汀和杂质A得到有效分离,分离度>1.5,流动相不干扰测定;左卡尼汀的检出限和定量限分别为15μg·L~(-1)和50μg·L~(-1),左卡尼汀杂质A的检出限为0.19μg·L~(-1);杂质A在质量浓度0.95~47.5μg·L~(-1)内线性关系良好(r=0.999 3)。结论建立的方法可用于左卡尼汀原料中有关物质的测定。 相似文献
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RP-HPLC法同时测定Beagle犬血浆中曲马多、文拉法辛和罗通定浓度 总被引:1,自引:0,他引:1
YU Qin ZOU Jing LIANG Mao-zhi NAN Feng QIN Yong-ping ZOU Yuan-gao 《药物分析杂志》2008,28(4):532-536
目的:建立同时测定 Beagle 犬血浆中曲马多、文拉法辛和罗通定浓度的反相高效液相色谱法。方法:Beagle 犬血浆标本以维拉帕米为内标,经碱化和石油醚-乙醚(7:3)提取后,以0.025 mol·L~(-1)磷酸二氢钠-甲醇(70:30)为流动相,流速1min·mL~(-1),经碳十八烷基键合硅胶柱(250 mm×4.6 mm,5μm)分离,采用荧光法于λ_(ex)=295 nm,λ_(em)=302 nm 检测。结果:曲马多标准曲线范围3.125~3200μg·L~(-1),Y=0.0051X 0.0473(r=0.9996),最低定量限为3.125μg·L~(-1),高、中、低3种浓度的日内精密度均<10%,日间精密度均<10%,方法回收率79.3%~111.2%;文拉法辛标准曲线范围6.25~1600μg·L~(-1),Y=0.0036X-0.0070(r=0.9998),最低定量限为6.25μg·L~(-1),高、中、低3种浓度的日内精密度均<7%,日间精密度均<6%,方法回收率92.5%~108.8%;罗通定标准曲线范围4.6875~2400μg·L~(-1),Y=0.0064X-0.0004(r=0.9999),最低定量限为4.6875μg·L~(-1),高、中、低3种浓度的日内精密度均<9%,日间精密度均<5%,方法回收率89.3%~112.1%。结论:本法简便、快速、准确,用于 Beagle 犬同时服用曲马多、文拉法辛和罗通定的药动学研究,取得满意结果。 相似文献
8.
目的探讨舒芬太尼对兔定量药物脑电图(QPEEG)β1频段的影响及其与阿片受体的关系。方法 36只成年家兔随机分为6组(n=6):空白组(0.9%Na Cl 1 m L·kg-1),低、中、高3个剂量舒芬太尼组(1.5,3,6μg·kg-1),纳洛酮组(400μg·kg-1)和联合用药组(纳洛酮400μg·kg-1+舒芬太尼3μg·kg-1)。采集给药前30 s及给药后1,3,5,10,20,25 min脑电图数据,分析QPEEG样本。结果与给药前相比,中、高剂量舒芬太尼组的β1频段功率百分比明显减少(P<0.05),且与舒芬太尼剂量呈负相关(P<0.05)。纳洛酮组与给药前相比,β1频段功率百分比无明显变化(P>0.05)。结论舒芬太尼以剂量依赖方式减少兔QPEEGβ1频段功率百分比,且此作用由阿片受体介导。 相似文献
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目的:建立高效液相色谱法测定围手术期患儿血浆瑞芬太尼浓度.方法:采用Hypersil CN柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.02 mol·L-1磷酸二氢钾水溶液内含三乙胺0.02%(30:70);流速1.0 ml·min-1;检测波长210nm;进样量为20 μl.结果:标准曲线在1.0~100.0 μg·L-1 内线性关系良好(r=0.999 3).最低检测浓度为1.0μg·L-1.提取回收率(76.51±0.82)%.方法回收率99.66%~102.40%.日内和日间RSD均小于15%.2μg·L-1组靶控浓度与实测浓度基本一致.结论:本方法快速、准确、灵敏、专一性好,适用于临床瑞芬太尼血药浓度检测和药动学研究. 相似文献
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目的比较不同方法快诱导全麻对减轻舒芬太尼诱发咳嗽反应的影响。方法 200例ASAI或Ⅱ级患者随机均分为4组,麻醉诱导方法分别为:Ⅰ组(对照组)依次静脉注射咪达唑仑0.05mg/kg、舒芬太尼0.4μg/kg、异丙酚1.5mg/kg、罗库溴胺1mg/kg;Ⅱ组(预注组)依次静脉注射咪达唑仑0.05mg/kg、舒芬太尼0.1μg/kg、异丙酚1.5mg/kg、罗库溴胺1mg/kg、舒芬太尼0.3μg/kg,Ⅲ组(稀释组)依次静脉注射咪达唑仑0.05mg/kg、舒芬太尼0.4μg/kg(2.5μg/mL)、异丙酚1.5mg/kg、罗库溴胺1mg/kg;Ⅳ组(后注射组)依次静脉注射咪达唑仑0.05mg/kg、异丙酚1.5mg/kg、罗库溴胺1mg/kg、舒芬太尼0.4μg/kg;除组Ⅲ外其余3组舒芬太尼浓度为10μg/mL。4组患者于诱导后2min进行气管插管,观察插管前咳嗽反应的发生率及严重程度,记录诱导前、诱导后、咳嗽时、插管时的SpO2、ABP和HR。结果 4组患者咳嗽的发生率Ⅱ组为8%(4/50),Ⅲ组为10%(5/50),Ⅳ组为2%(1/50),Ⅱ、Ⅲ、Ⅳ组明显低于Ⅰ组的38%(19/50)(P<0.01),Ⅱ、Ⅲ组低于Ⅳ组(P<0.05);4组患者T1、T2、T3、T4时间点的SBP和HR差异无统计学意义;T3的SBP、HR均较T1、T2明显升高(P<0.01)。结论快速诱导全身麻醉时舒芬太尼最后给药、稀释给药或给予预注剂量均可以明显降低舒芬太尼诱发咳嗽反应的发生率,其中以最后给药效果最佳。 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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《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
16.
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
17.
《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
18.
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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