高效液相色谱法测定匹林咖敏片中3组分的含量

目的:采用高效液相色谱法同时测定匹林咖敏片中3组分咖啡因、阿司匹林和马来酸氯苯那敏的含量。方法:色谱柱为ZORBAX Eclipse XDB-C_(18)(150mm×4.6mm,5μm),流动相为甲醇-4.3%冰醋酸溶液(17:83),柱温30℃,流速为1.0ml·min~(-1),检测波长为262nm。结果:咖啡因、阿司匹林和马来酸氯苯那敏的线性范围分别为:3.2～50.6μg·ml~(-1)(r=1.000 0)、24.5～392μg·ml~(-1)(r=1.000 0)和0.4～6.6μg·ml~(-1)(r=0.999 9);平均回收率分别为99.2%,99.3%,99.5%,RSD分别为1.1%,0.7%,0.6%。结论:方法快速、简便,适用于控制药品质量。     

高效液相色谱法同时测定大黄碳酸氢钠片中5种成分的含量

目的建立高效液相色谱法测定大黄碳酸氢钠片中5种成分的含量。方法采用Agilent Eclipse XDB-C18(4.6 mm×250 mm,5μm)色谱柱;以乙腈(A)-0.1%磷酸溶液(B)为流动相梯度洗脱,检测波长为254 nm;柱温为30℃;流速1.0 mL·min~(-1)。结果芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚分别在3.488～34.875μg·mL~(-1)(r=0.9996)、3.010～30.100μg·m L~(-1)(r=0.9997)、4.566～45.660μg·mL~(-1)(r=0.9996)、3.236～32.357μg·mL~(-1)(r=0.9996)、1.867～18.671μg·mL~(-1)(r=0.9981)与峰面积呈良好的线性关系,加样回收率分别为96.8%、98.3%、99.7%、101.4%、103.2%,RSD分别为2.4%、2.5%、1.9%、1.8%、0.76%。结论该实验方法准确性可靠、重复性和稳定性良好,专属性强,可作为大黄碳酸氢钠片含量测定的质控方法。     

HPLC法测定牛黄清火丸中大黄素和大黄酚的含量

目的:建立牛黄清火丸的含量测定方法。方法:采用高效液相色谱法。色谱柱:SHIMADZU VP-ODS(250 mm×4.6 mm,5μm),流动相:甲醇-0.1%磷酸溶液(80:20,V/V),流速:1.0ml·min~(-1),检测波长:254 n nm,柱温:30℃。结果:大黄素在10.04～50.20μg·ml~(-1)范围内线性关系良好(r=0.999 8);平均加样回收率为98.0%,RSD=1.5%(n=6);大黄酚在20.04～60.12μg·ml~(-1)范围内线性关系良好(r=1.0000);平均加样回收率为99.2%,RSD 1.1%(n=6)。结论:该方法简便易行,结果准确可靠,可适用于牛黄清火丸的质量控制。     

超高效液相色谱法同时测定活血涤痰汤中7种活性成分的含量

目的建立UPLC方法同时测定活血涤痰汤中黄芪甲苷、柴胡皂苷a、柴胡皂苷d、大黄酸、大黄素、大黄酚和大黄素甲醚含量。方法采用Waters BEH C18色谱柱(2.1 mm×50 mm,1.7μm),流动相为乙腈(A)-0.1%磷酸水溶液(B),梯度洗脱,体积流量为0.3 mL·min~(-1),进样量为3μL,检测波长分别为205和254 nm。结果黄芪甲苷、柴胡皂苷a、柴胡皂苷d、大黄酸、大黄素、大黄酚、大黄素甲醚的线性范围分别为2.89～57.76μg·m L~(-1)(r=0.9993)、2.10～42.08μg·m L~(-1)(r=0.9994)、3.04～60.88μg·m L~(-1)(r=0.9993)、1.06～21.12μg·m L~(-1)(r=0.9998)、0.89～17.84μg·m L~(-1)(r=0.9999)、1.18～23.60μg·m L~(-1)(r=0.9999)、1.14～22.88μg·m L~(-1)(r=0.9998),平均加样回收率分别为97.5%,97.3%、98.2%、99.3%、99.1%、99.1%和98.8%,RSD值分别为2.4%、2.5%、2.0%、2.0%、2.1%、2.1%和1.9%。结论建立的UPLC方法简便快速,重现性好,可用于活血涤痰汤的质量控制与评价。     

多种药材与制剂中大黄酚与大黄素含量测定改进方法

目的:改进大黄酚与大黄素的测定方法。方法:通过甲醇提取与酸水解同步进行,用高效液相色谱法简便、快捷、准确地测定了多种药材与制剂中大黄酚与大黄素含量。色谱条件为:Shimadzu VP—ODS C_(18)(150 mm×4.6 mm,5μm)为色谱柱,甲醇-0.1%磷酸(85:15)为流动相,流速:1.0 mL·min~(-1),检测波长为254 nm。结果:通过方法学考察,大黄酚的进样量在0.022～0.32μg(r=0.9999),大黄素的进样量在0.015～0.22μg(r=0.9999)范围内,呈良好的线性关系。大黄酚与大黄素的平均回收率(n=3)分别为96.10%～101.7%和96.75%～100.9%。结论:改进方法检测效率高,检测成本低,环境污染轻。     

HPLC测定复方陈香胃片中的大黄素、大黄酚和大黄素甲醚

目的 采用HPLC法测定复方陈香胃片中大黄素、大黄酚和大黄素甲醚的含量。方法 采用Kromasil 100-5-C₁₈色谱柱(250 mm×4.6 mm, 5μm),流动相为乙腈-甲醇-0.4%磷酸溶液(40:25:35),检测波长为254 nm,进样量10μL。结果 0.3951-9.8784μg·mL^-1大黄素、4.1986-104.97μg·mL^-1大黄酚、0.8547-21.3677μg·mL^-1大黄素甲醚与峰面积的线性关系良好,r均为0.9999平均回收率分别为101.7%、101.7%、103.2%,RSD分别为2.50%、2.71%、2.77%(n=9)。结论 所用方法低毒、简便、准确、重复性好,可用于复方陈香胃片的质量控制。     

HPLC测定一清颗粒中大黄素和大黄酚的含量

目的建立一清颗粒中大黄素和大黄酚的含量测定方法.方法采用HPLC法进行测定,色谱柱为Dikma C18(250mm×4.6 mm,5μm);流动相为甲醇-0.1%磷酸(8515);检测波长为254 nm柱温25℃.结果一清颗粒中大黄素和大黄酚的的线性范围分别为3.28-32.80μg·ml-1,7.12～71.20μg·ml-1,r=0.999 9.大黄素平均回收率为96.47%,RSD1.4%;大黄酚平均回收率为98.26%,RSD 0.87%.结论该方法简便,结果准确,重现性好,可作为一清颗粒的质量控制方.法.     

HPLC法测定复方甘草酸苷胶囊中三组分的含量

目的:采用HPLC法测定复方甘草酸苷胶囊3组分的含量。方法:甘草酸苷:用ODS-C_(18)柱(150 mm×4.6 mm,5μm);2%冰醋酸-乙腈(65:35)为流动相,流速为1.0 ml·min~(-1),检测波长为252 nm;甘氨酸和蛋白酸:采用2,4-硝基氟苯柱前衍生化方法,色谱柱ODS C_(18)(250 mm×4.6 mm,5μm);乙腈-0.05 mol·L~(-1)醋酸钠缓冲液(35:65),检测波长:360 nm,流速1.0 ml·min~(-1)。结果:甘草酸苷、甘氨酸和蛋氨酸的线性范围分别为103.3～826.7μg·ml~(-1)(r=0.999 8),6.25～50.0μg·ml~(-1) (r=0.999 5)和6.33～50.67μg·ml~(-1)(r=0.999 5),其回收率分别为99.8%,99.7%和99.8%,RSD分别为0.3%,0.3%和0.4 (n=9)。结论:该法简便、灵敏、准确。     

RP-HPLC测定热灼平喷雾剂中的大黄酸、大黄素和大黄酚

目的 采用RP-HPLC法测定热灼平喷雾剂中的大黄酸、大黄素、大黄酚.方法采用Luna-C18色谱柱(150mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸(80:20),柱温25°C,流速1.0 ml·min-1,检测波长254 nm.结果 大黄酸、大黄素、大黄酚的线性范围分别为85.2～852.0μg(r=0.9999)、88.0～880.0μg(r=0.9998)、107.2～1072.0μ g(r=0.9999),平均回收率分别为99.88%(RSD=3.02%)、105.0%(RSD=2.45%)、102.5%(RSD=1.48%).结论 所建方法简便、准确.     

青翘片中阿司匹林的含量测定

目的:建立青翘片中阿司品林含量测定方法。方法:色谱柱:Shim-pack CLC C_(18)(150 mm×4.6 mm,5μm);流动相:乙腈:0.08 mol·L~(-1)醋酸钠溶液(冰醋酸调pH至3.65)(15:85),流速:2 ml·min~(-1),检测波长:230 nm。紫外分光光度法检测波长:300 nm。结果:高效液相法:阿司匹林的线性范围为2～10μg·ml~(-1)(r=0.9999),回收率100.5%,RSD为0.8%(n= 6)。紫外分光光度法:阿司匹林在5～30μg·ml~(-1)呈线性,平均回收率为100.9%,RSD为0.6%(n=5)。结论:两种方法均适用于青翘片中阿司匹林的含量测定。     

Efficacy of gut lavage,hemodialysis, and hemoperfusion in the therapy of paraquat or diquat intoxication

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.

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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.

     

In vitro studies on sterically stabilized liposomes (SL) as enzyme carriers in organophosphorus (OP) antagonism

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.     

Aquatic Insects and Trace Metals: Bioavailability,Bioaccumulation, and Toxicity

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.     

Steroidal sapogenin contents in some domestic plants

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.     

Alzheimer’s disease – current trends in basic and clinical research. Highlights from the 16th ECNP

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.