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1.
目的 建立高效液相色谱法测定壮骨颗粒中补骨脂素和异补骨脂素的含量。方法 色谱柱为Agilent Zorbax C18柱(4.6 mm×250 mm,5 μm),流动相为甲醇-水(45:55),检测波长为245 nm,流速为1.0 ml/min,柱温为25 ℃,进样量为10 μl。采用70%乙醇水浴方法提取壮骨颗粒中的补骨脂素和异补骨脂素。结果 补骨脂素与异补骨脂素在3.75~40 μg/ml范围内呈良好的线性关系,对方法精密度(n=6)、重复性(n=6)和稳定性(12 h)进行考察,相对标准偏差(RSD)均小于2%。加样回收率(n=6)为94%~105%。结论 该测定方法简便、快速、准确,可用于壮骨颗粒的临床快速质量控制。  相似文献   

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目的 建立高效液相色谱法测定田七痛经胶囊中阿魏酸、藁本内酯、欧当归内酯A的方法。方法 选用Thermo Acclaim C18色谱柱,Thermo SCIENTIFICSyncronis C18色谱柱;检测波长为321、280 nm;体积流量1.0 mL/min;柱温35℃结果 阿魏酸、藁本内酯、欧当归内酯A的质量浓度与峰面积分别在1.12~112.30、1.33~132.60、0.96~95.50 μg/mL呈良好的线性关系;回归方程分别为Y=46 335 540 X+44 186.71(r=0.998),Y=14 514 060 X+8 715.27(r=0.999),Y= 22 031 250 X+16 472.10(r=0.999)。结论 该方法准确,简便,灵敏,可作为田七痛经胶囊质量控制的方法。  相似文献   

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目的 采用多波长HPLC法建立仙灵骨葆胶囊中淫羊藿苷、朝藿定C、川续断皂苷Ⅵ、补骨脂素及异补骨脂素的含量测定方法。方法 采用月旭Ultimate® XB-C18柱,流动相采用乙腈-水系统,梯度洗脱;柱温:30 ℃;检测波长:淫羊藿苷、朝藿定C、川续断皂苷Ⅵ为212 nm,补骨脂素、异补骨脂素为246 nm。结果 5种成分均能达到基线分离,各成分的进样量分别在:淫羊藿苷0.008 2~0.328 μg(r=0.999 5)、朝藿定C 0.055 6~2.224 μg(r=0.999 6)、川续断皂苷Ⅵ 0.144 1~5.764 μg(r=0.999 6)、补骨脂素0.005 4~0.215 2 μg(r=0.998 0)、异补骨脂素0.006 6~0.265 6 μg(r=0.998 5)范围内线性关系良好,平均回收率分别为97.59%、98.58%、98.11%、97.86%、98.22%,RSD均小于2.0%。结论 该方法操作简便、分离良好、数据准确、灵敏度高,可用于仙灵骨葆胶囊的多指标成分定量测定。  相似文献   

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目的 以西咪替丁为内标,建立RP-HPLC法测定盐酸左旋咪唑片的含量。方法 选用ODS-C18柱(5μm,4.6mm×150mm);流动相:甲醇-水-二乙胺-磷酸(36∶64∶0.1∶0.06),pH7.0;检测波长:215nm;流量∶1.0ml·min-1;进样体积∶20μl。结果 进样量在0.32~1.6μg范围内,相关性良好,回归方程:Y=22.01X+7.4×10-3,r=0.9998。平均回收率为99.8%(n=5)。结论 本法简便、快速、准确。  相似文献   

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目的 建立高效液相色谱法测定祛痰合剂中橙皮苷的含量。方法 采用Agilent Eclipse XDB-C18柱(250 mm×4.6 mm,5 μm),流动相为甲醇-冰醋酸-水(25∶5∶70),流速1 mL·min-1,检测波长283 nm,柱温30 ℃。结果 橙皮苷线性范围是1.05~34.56 μg·mL-1,线性方程为Y=10.346X+0.795 2,r=0.999 6;平均回收率为98.8%,RSD为1.2%(n=9) 。结论 本法简便,准确和选择性好,可用于祛痰合剂的质量控制。  相似文献   

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目的 建立斑蝥酸钠维生素B6注射液中斑蝥酸钠和维生素B6含量的同时测定方法。方法 采用HPLC,色谱柱为Syncronis C18(250 mm×4.6 mm,5 μm),流动相为0.02 mol·L-1磷酸二氢钾溶液(磷酸调pH值至2.6)-乙腈,梯度洗脱,流速为1.0 mL·min-1,检测波长为193,290 nm,波长切换法,柱温:30℃。结果 斑蝥酸钠回归方程为Y=1.926X+0.010(r=0.999 7),在0.064 6~0.322 8 mg·mL-1内斑蝥酸钠与峰面积的线性关系良好,平均回收率为98.9%,RSD为1.2%(n=9)。维生素B6回归方程为Y=24.153X+0.670(r=0.999 9),在0.535 9~2.679 7 mg·mL-1内维生素B6与峰面积的线性关系良好,平均回收率为100.2%,RSD为1.0%(n=9);仪器精密度、稳定性和重复性试验的RSD均<2.0%。结论 所建立的方法结果准确、重复性好,可用于斑蝥酸钠维生素B6注射液的质量控制。  相似文献   

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目的 基于细胞色素P450(CYP450)代谢酶探究补骨脂素和异补骨脂素对黄独乙素在大鼠体内代谢的影响。方法 采用大鼠离体循环肝灌流方法,考察大鼠分别给予补骨脂素或异补骨脂素1、3、7 d后,黄独乙素在肝脏中的代谢情况;利用UPLC-MS/MS检测循环灌流液中剩余黄独乙素的含量;通过大鼠眼内眦取血的方法研究大鼠分别给予补骨脂素或异补骨脂素干预1周,再给予黄药子提取物(10 g·kg-1)后体内黄独乙素的药动学变化,药动学参数采用DAS 2.0软件中的非房室模型法进行计算。结果 大鼠给予补骨脂素或异补骨脂素后,循环灌流液中黄独乙素的含量相对增加,且补骨脂素或异补骨脂素给药时间延长后,对酶的抑制程度更强;当大鼠给予补骨脂素或异补骨脂素干预后,与非干预组(黄药子提取物组)相比,药时曲线下面积(AUC0~t)和平均驻留时间(MRT0~t)增加,消除半衰期(t1/2Z)减小。结论 补骨脂素/异补骨脂素可通过抑制肝脏中CYP450酶的活性降低其对黄独乙素的代谢,使黄独乙素在肝脏中代谢减少,造成蓄积,临床用药应注意含有补骨脂素/异补骨脂素或黄独乙素中药在合用时可能产生的药物相互作用。  相似文献   

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克白合剂质量标准提升研究   总被引:1,自引:1,他引:0  
目的 完善并提升克白合剂的质量标准。方法 以黄芪甲苷作为指标成分建立薄层色谱鉴别法。采用HPLC建立补骨脂素、异补骨脂素的含量测定方法,对10批克白合剂进行定性定量检测,拟定克白合剂质量标准草案。结果 薄层色谱斑点清晰,分离度好;补骨脂素在1.41~45.20 μg·mL-1r=1.000 0)、异补骨脂素在1.30~41.40 μg·mL-1r=1.000 0)内与峰面积呈良好的线性关系。补骨脂素和异补骨脂素的平均回收率分别为98.1%,98.3%,RSD分别为0.6%,0.6%(n=6)。结论 从克白合剂10批样品数据综合分析,建议克白合剂每1 mL含补骨脂和异补骨脂素的总量≥ 38.0 μg,质量标准体系的提升为临床用药提供了更可靠的质量保证。  相似文献   

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目的 建立同时测定栀子中3种环烯醚萜苷类成分含量的方法。方法 采用液相色谱-串联质谱(LC-MS/MS)法。色谱条件:Dikma Diamonsil® C18柱(100 mm×4.6 mm,5 μm);流动相为0.1%乙酸水(A)-0.1%乙酸乙腈(B),梯度洗脱;流速为0.4 ml/min;柱温40℃;进样量2 μl。质谱条件:电喷雾离子化电离源(ESI),正/负离子检测,雾化气流量3 L/min,干燥气流量15 L/min,脱溶剂管温度240℃,加热块温度400℃,碰撞气压力230 kPa,以多反应监测模式(MRM)配对离子方式进行定量,山栀苷、京尼平龙胆双糖苷、栀子苷选择的离子对质荷比分别为m/z 391.10→149.30,m/z 573.40→365.05,m/z 447.30→225.15。结果 回归方程为:山栀苷Y=243.810X-289.957,r=0.999 9;京尼平龙胆双糖苷Y=137.125X+2 092.76,r=0.999 6;栀子苷Y=2 030.32X+823 213,r=0.999 8;线性范围分别为10.76~2 152 ng/ml、516~4 128 ng/ml、2 000~20 000 ng/ml。精密度、稳定性、重复性和加样回收率试验结果均符合要求。结论 此方法可快速、准确、灵敏地测定栀子中3种环烯醚萜苷类成分的含量,为栀子的质量控制提供依据。  相似文献   

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目的 建立康得灵胶囊中黄芩苷的HPLC测定方法。方法 色谱柱为Agilent Tc-C18色谱柱(4.6 mm×250 mm,5 μm),柱温为30 ℃;流动相为乙腈-0.5‰磷酸溶液(26:74),流速为1.0 ml/min,检测波长265 nm。结果 黄芩苷保留时间约为16 min。以峰面积(Y)对进样浓度(X, μg/ml)线性回归,得回归方程:Y=22 114.67 X-112 836.7,r=0.998 8,线性范围5.410~108.2 μg/ml。平均加样回收率为98.78%,RSD为0.74%。结论 本方法操作简便,测定结果准确可靠,可用于康得灵胶囊中黄芩苷的含量测定。  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.
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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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Abstract

The 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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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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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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