高效液相色谱法测定苦荞籽壳中芦丁和槲皮素的含量

目的:建立高效液相色谱法测定苦荞籽壳中芦丁和槲皮素的含量。方法:采用 Zorbax SB-C_(18)(4.6 mm×150 mm,5μm)色谱柱;流动相为甲醇-0.4%磷酸(50:50);流速1.0 mL·min~(-1);检测波长254 nm。结果:芦丁进样量在0.024～0.963mg·mL~(-1)范围内(r=0.9996),槲皮素进样量在0.0132～0.528 mg·mL~(-1)范围内(r=0.9990)线性关系良好,平均回收率芦丁为100.1%(RSD=1.15%),槲皮素为99.9%(RSD=1.04%)。结论:该方法操作简便,分离度高,重复性好,可同时测定苦荞籽壳中芦丁和槲皮素的含量。     

高效液相色谱分离柱后化学发光法同时测定菟丝子中黄酮类成分

目的:建立高效液相色谱分离柱后化学发光法测定菟丝子中芦丁、山柰素、槲皮素和异鼠李素含量。方法:基于在氢氧化钠碱性介质中铁氰化钾可以直接氧化芦丁、山柰素、槲皮素和异鼠李素产生化学发光。色谱柱:Hypersil ODS(5μm,4.6 mm×150 mm),流动相:乙醇-乙腈-水-磷酸(21:22:55:2),流速:1mL·min~(-1),柱温:25℃。结果:芦丁、山柰素、槲皮素和异鼠李素浓度分别在0.2～5μg·mL~(-1)(r=0.9990),0.1～15μg·mL~(-1)(r=0.9991),0.1～100μg·mL~(-1)(r=0.9994),0.3～200μg·mL~(-1)(r=0.9998)范围内,与峰面积有良好的线性关系;检测限(S/N=3)分别为0.02,0.08,0.08,0.03μg·mL~(-1)。结论:水法简便、快速、有效,灵敏度高,首次用于菟丝子中黄酮类成分的测定,取得了很好的结果。     

RP—HPLC法测定鲜人参中丙二酰基人参皂苷的含量

目的:建立人参中丙二酰基人参皂苷含量的测定方法。方法:采用反相高效液相色谱法,以μ-Bondapak C-18(300mm×3.9 mm,5 μm)柱为分析柱,乙腈-0.05 mol·L~(-1)磷酸二氢钾溶液(25:75)为流动相,柱温:35℃,检测波长:203 nm,流速:1 mL·min~(-1),以外标法检测。结果:丙二酰基人参皂苷 Rb_1、Rb_2、Rc 分别在0.02～1.19 mg·mL~(-1)(r=0.9998)、0.02～0.99 mg·mL~(-1)(r=0.9997)、0.01～0.83 mg·mL~(-1)(r=0.9996)浓度范围内呈良好的线性关系。平均回收率(n=3)分别为103.0%(RSD=1.3%)和98.5%(RSD=1.0%)、102.4%(RSD=1.2%)和98.1%(RSD=0.6%)、102.1%(RSD=2.8%)和100.1%(RSD=1.0%)。结论:本法简便、准确、灵敏。     

HPLC法同时测定天山雪莲中紫丁香苷、绿原酸和芦丁的含量

目的:采用液相色谱法同时测定天山雪莲中紫丁香苷、绿原酸和芦丁的含量。方法:Kromasil ODS-1色谱柱(250 mm×4.6 mm,5μm),柱温为35℃;以乙腈(A)-0.4%磷酸(B)为流动相,梯度洗脱(0 min,13%A;15 min,13%A;16 min,15%A;40 min11,15%A),流速1 mL·min~(-1);双波长检测:257 nm(检测紫丁香苷、芦丁),327 nm(检测绿原酸)。结果:紫丁香苷存5.104～51.04 μg·mL~(-1)(r=0.9998)、绿原酸在38.82～258.8μg·mL~(-1)(r=0.9991)、芦丁在39.42～262.8μg·mL~(-1)(r=0.9997)范围内都呈良好线性关系;紫丁香苷、绿原酸和芦丁的回收率分别为99.7%(RSD=1.0%),102.9%(RSD=1.5%),101.7%(RSD=1.2%);供试品溶液在12 h 内稳定。结论:该方法快速简单,线性关系良好。     

HPLC法同时测定复方氨酚苯海拉明片中4种成分的含量

目的:建立高效液相色谱法同时测定复方氨酚苯海拉明片中对乙酰氨基酚、咖啡因、盐酸苯海拉明和盐酸麻黄碱的含量。方法:采用迪马 C_(18)色谱柱(200 mm×4.6mm,5 μm);流动相为乙腈(A)-水(磷酸调节 pH 至2.1)(B),梯度洗脱[0 min(15%A)→7 min(50%A)→8 min(15%A)→18 min(15%A)];流速:1.0 mL·min~(-1);检测波长:215 nm;柱温:室温。结果:对乙酰氨基酚、咖啡因、盐酸苯海拉明和盐酸麻黄碱的线性范围分别为0.064～0.51 mg·mL~(-1)(r=0.9999)、0.067～0.54 mg·mL~(-1)(r=0.9995)、0.020～0.14 mg·mL~(-1)(r=0.9998)和0.017～0.14 mg·mL~(-1)(r=0.9999);平均回收率分别为100.1%(RSD=0.5%)、99.6%(RSD=0.8%)、101.4%(RSD=1.0%)和99.2%(RSD=0.6%)。结论:本法简便快速,结果准确可靠,可作为该复方制剂中4种成分的质量控制方法。     

HPLC双波长法同时测定意大利牛舌草中3种成分的含量

目的建立同时测定意大利牛舌草中咖啡酸、芦丁和紫云英苷含量的HPLC法。方法采用πNAP COSMOSIL C18色谱柱(250mm×4.6mm,5μm);以乙腈(A)-2mL·L-1磷酸(B)为流动相,进行梯度洗脱;流速:1.0mL·min~(-1);柱温:30℃;紫云英苷、咖啡酸和芦丁的检测波长分别为266,341和341nm。结果咖啡酸、芦丁和紫云英苷分别在0.348 8~22.32(r=0.999 9),1.813~116.0(r=0.999 9)和0.241 3~15.44μg·mL~(-1)(r=0.999 8)范围内质量浓度与峰面积线性关系良好,平均回收率分别为99.6%(RSD=1.28%),101.1%(RSD=0.66%)和99.8%(RSD=3.75%)。3批意大利牛舌草样品中咖啡酸、芦丁和紫云英苷的平均含量分别为84.27±2.19,720.77±62.85和63.63±4.33μg·g~(-1)。结论该方法操作简便、重复性好、准确度高,为意大利牛舌草的质量控制提供了实验依据。     

RP-HPLC法测定新疆哈萨克族常用药材包尔胡特果实中芦丁和槲皮素的含量

目的建立测定新疆包尔胡特(Rhamnus cathartica L.)果实中芦丁和槲皮素含量的方法。方法色谱柱:依利特Hypersil ODS2C18(260mm×4.6mm,5μm)配预柱;芦丁的流动相:甲醇-10mL·L~(-1)乙酸溶液(70∶30),槲皮素的流动相:甲醇-4mL·L~(-1)磷酸溶液(35∶65);流速均为1.0mL·min~(-1);柱温:30℃;芦丁检测波长:257nm,槲皮素检测波长:360nm;进样量均为10μL。结果芦丁质量浓度在43.411 0~165.600 0μg·mL~(-1)范围内线性关系良好(r=0.999 7),平均加样回收率为99.84%,RSD值为1.45%;槲皮素质量浓度在5.454 0~87.264 0μg·mL~(-1)范围内线性关系良好(r=0.999 9),平均加样回收率为99.83%,RSD值为1.49%。结论该方法简便、准确、重复性好,可用于包尔胡特果实原料中芦丁和槲皮素的含量测定。     

HPLC法同时测定当归药材中6种成分的含量

目的:建立高效液相色谱法同时测定当归药材中阿魏酸、阿魏酸松柏酯、Z 型和 E 型藁本内酯及 Z 型和 E 型3-丁烯基苯酞的含量。方法:采用 Zorbax ODS C_(18)色谱柱(250 mm×4.6 mm,5 μm);流动相为1%醋酸(A)-乙腈(B),梯度洗脱(0min,10%B;7 min,33%B;55 min,33%B),流速1.0 mL·min~(-1);检测波长为324 nm(阿魏酸、阿魏酸松柏酯和 Z/E 型藁本内酯)和260 nm(Z 型和 E 型3-丁烯基苯酞)。结果:阿魏酸、阿魏酸松柏酯、Z-藁本内酯、Z 型和 E 型3-丁烯基苯酞的线性范围分别为3.31～139.50 μg·mL~(-1)(r=0.9999),38.00～380.00 μg·mL~(-1)(r=0.9995),2.11～445.00 μg·mL~(-1)(r=1.000),3.32～136.18 μg·mL~(-1)(r=0.9999),1.94～16.32 μg·mL~(-1)(r:0.9995);加样回收率分别为101.8%(RSD=2.5%),105.3%(RSD=3.2%),98.5%(RSD=1.6%),105.3%(RSD=2.4%),105.8%(RSD=1.9%)。结论:该方法准确、简便,具有良好的重复性和稳定性,有利于提高当归药材的质量控制。     

不同来源鱼腥草中槲皮素含量差异比较研究

目的:建立 RP-HPLC 法,比较不同来源鱼腥草中槲皮素含量差异。方法:采用高效液相色谱法,色谱柱:Hypersil ODSC_(18)柱(4.0 mm×250 mm,5μm),流动相:乙腈-0.4%磷酸(pH 3.0)(45:55),流速1.0 mL·min~(-1),柱温30℃,紫外检测波长370 nm。结果:槲皮素含量在0.0224～2.24μg范围内具有良好的线性关系(r=0.9997)。低、中、高回收率(n=3)分别为102.4%,99.78%,101.4%;RSD 分别为3.6%,0.96%,1.7%。W01-120号鱼腥草中槲皮素含量水平最高,达4.02 mg·g~(-1)。结论:该方法简便、快速、准确,不同来源的鱼腥草间槲皮素含量差异显著。     

夏枯草中齐墩果酸和熊果酸的含量测定方法研究

目的通过采用高效液相色谱法,测定不同产地夏枯草中齐墩果酸和熊果酸的含量,比较夏枯草药材质量的优劣。方法色谱柱:Kromasil-C_(18)(250 mm×4.6 mm,5μm);流动相:乙腈-甲醇-0.2%磷酸水(5∶82∶13)等度洗脱;流速:1.0 mL·min~(-1);检测波长:210 nm;柱温:25℃。结果齐墩果酸在0.041~0.410 mg·mL~(-1)与峰面积呈现良好的线性关系(r=0.9999),平均回收率为99.1%,RSD为1.8%;熊果酸在0.054~0.540 mg·mL~(-1)与峰面积呈现良好的线性关系(r=0.9998),平均回收率为98.1%,RSD为2.4%。结论该方法简单、准确、可靠,为夏枯草的质量控制与评价提供了有效的手段。     

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.