HPLC-PDA法同时测定更年宁中芍药苷、阿魏酸、黄芩苷和丹皮酚的含量

目的建立HPLC-PDA法同时测定更年宁中芍药苷、阿魏酸、黄芩苷和丹皮酚的含量。方法采用Phenomsil C18(4.6 mm×250 mm,5μm)色谱柱;流动相:以乙腈为流动相A,以0.15%磷酸为流动相B,采用梯度洗脱;流速为1.0 mL·min~(-1);柱温为35℃;芍药苷的检测波长为230 nm,阿魏酸的检测波长为320 nm,黄芩苷的检测波长为280 nm,丹皮酚的检测波长为274 nm。结果芍药苷、阿魏酸、黄芩苷、丹皮酚浓度分别在5.077～50.77、0.297～2.97、8.976～89.76、3.37～33.70μg·mL~(-1)与峰面积线性关系良好,平均回收率分别为98.5%(RSD=0.83%)、98.4%(RSD=1.5%)、98.9%(RSD=1.1%)、98.4%(RSD=1.0%)。结论该方法简便、灵敏、结果准确可靠,可为其提高质量控制标准提供参考。     

HPLC法同时测定女金胶囊中黄芩苷和丹皮酚的含量

目的:高效液相色谱法测定女金胶囊中黄芩苷和丹皮酚的含量.方法:色谱柱:Symmetry C18柱(150 mm×3.9 mm,5μm);流动相:甲醇-0.4％磷酸(48∶52),流速:1ml ·min-1;紫外检测波长:276 nm;柱温:30℃;进样量:10μl.结果:在4.96～24.80 μg和2.60～13.00 μg范围内成线性关系,平均回收率分别为98.3％和98.4％(n=6).结论:该方法简便,准确,可作为女金胶囊中黄芩苷和丹皮酚含量的测定方法.     

高效液相色谱法同时测定安坤胶囊中栀子苷、芍药苷、特女贞苷、蟛蜞菊内酯和丹皮酚的含量

目的建立HPLC法同时测定安坤胶囊中栀子苷、芍药苷、特女贞苷、蟛蜞菊内酯和丹皮酚含量。方法采用Agilent TC-C18色谱柱(4.6 mm×250 mm,5μm),流动相:乙腈-0.1%磷酸水溶液,梯度洗脱;检测波长230 nm(0～30 min)、351 nm(30～40 min)、274 nm(40～50 min);流速1.0mL·min~(-1);柱温30℃,进样量:10μL。结果栀子苷、芍药苷、特女贞苷、蟛蜞菊内酯和丹皮酚分别在81.83～4091.69 ng(r=0.9999)、79.71～3985.61 ng(r=0.9999)、15.58～778.91 ng(r=0.9999)、1.35～67.40 ng(r=0.9992)、16.54～827.20 ng(r=0.9998)与峰面积线性关系良好;平均回收率分别为98.5%、97.2%、97.9%、102.9%、97.6%,RSD值分别为0.80%、1.0%、1.6%、2.6%、1.9%。结论该方法简便、快速、重复性好,可用于安坤胶囊的质量控制。     

超高效液相色谱法同时测定白芍中芍药苷和芍药内酯苷的含量

目的 采用超高效液相色谱法(UPLC)同时测定白芍中芍药苷和芍药内酯苷的含量.方法 采用Agilent Extend-C18(4.6 mm×50 mm,1.8μm)色谱柱,以流动相乙腈(A)-0.2％乙酸溶液(B)梯度洗脱;柱温30℃;流速0.5 mL·min-1;检测波长230 nm.结果 芍药苷和芍药内酯苷分别在0.011 6～1.45(r=0.999 9)、0.008～lmg·mL-1(r=0.999 9)呈良好的线性关系;平均回收率分别为98.6％、97.5％,RSD分别为1.4％、2.2％.结论 该法快速简便,灵敏度高,准确可靠,可用于白芍中有效成分含量的快速测定及白芍的质量控制.     

超高效液相色谱法同时测定丹蛭降糖胶囊中丹皮酚和芍药苷含量

目的:建立一种超高效液相色谱法同时测定丹蛭降糖胶囊中丹皮酚、芍药苷的含量。方法:色谱柱为Waters Acquity UPLC BEH C18(50 mm×2.1 mm,1.7μm)柱,以乙腈-0.1%磷酸为流动相进行梯度洗脱,流速为0.25 mL.min-1,柱温为30℃,检测波长为230 nm。结果:丹皮酚和芍药苷的线性范围分别为0.653～1.959μg(r=0.999 7)和0.108～0.324μg(r=0.999 9),平均加样回收率分别为99.46%,RSD=0.46%(n=6)和99.19%,RSD=0.49%(n=6)。结论:新建方法简便、快速、准确、易行,可用于控制制剂质量。     

HPLC法双波长同时测定赤芍中4种成分的含量

目的：采用高效液相色谱法,在不同检测波长下同时测定赤芍中儿茶素、芍药苷、苯甲酸、丹皮酚4种成分的含量。方法色谱柱为DiamonsilC185μm250＆#215;4.6mm,以0.1%甲酸-乙腈为流动相进行梯度洗脱,检测波长为230nm（儿茶素、芍药苷、苯甲酸）,275nm（丹皮酚）,流速1mL·min-1,柱温30℃。结果不同产地赤芍中4种成分含量差异较大,7批不同产地赤芍药材中儿茶素、芍药苷、苯甲酸和丹皮酚的含量范围分别为：0%-0.052%、1.044%-4.326%、0.126%-0.249%、0.022%-1.060%。结论本法操作简便、准确、重复性好,可用于赤芍药材中儿茶素、芍药苷、苯甲酸、丹皮酚含量的测定。     

六味地黄丸中四种活性成分的HPLC法测定

建立了HPLC法同时测定六味地黄丸中的丹皮酚、马钱苷、莫诺苷和芍药苷.采用C_(18)色谱柱,以乙腈-0.1%磷酸溶液梯度洗脱,检测波长238 nm,丹皮酚、马钱苷、莫诺苷和芍药苷分别在0.5～20、0.25～10、0.5～20和0.15～6μg/ml浓度范围内线性关系良好,回收率分别为98.10%～105.44%.     

HPLC波长切换法同时测定白芍饮片中9个成分的含量

目的:建立高效液相色谱波长切换法对白芍中9个成分(没食子酸、氧化芍药苷、儿茶素、芍药内酯苷、芍药苷、苯甲酸、1,2,3,4,6-五没食子酰葡萄糖、苯甲酰芍药苷、丹皮酚)进行分析。方法:采用Phenomsil ODS(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-0.1%磷酸水(B)为流动相,梯度洗脱,流速1.0 mL.min-1,检测波长为267 nm(0～12 min,测定没食子酸)、258 nm(12～30 min,测定氧化芍药苷、儿茶素)、230 nm(30～38 min,测定芍药内酯苷、芍药苷)、223 nm(38～42 min,测定苯甲酸)、275 nm(42～56 min,测定1,2,3,4,6-五没食子酰葡萄糖)、230 nm(56～70 min,测定苯甲酰芍药苷、丹皮酚)。结果:白芍中9个成分没食子酸、氧化芍药苷、儿茶素、芍药内酯苷、芍药苷、苯甲酸、1,2,3,4,6-五没食子酰葡萄糖、苯甲酰芍药苷、丹皮酚进样量分别在0.13～0.87μg(r=0.9991),0.13～0.85μg(r=0.9991),2.50×10-3～17.50×10-3μg(r=0.9993),0.26～1...     

HPLC-MS/MS法同时测定脑血疏口服液中三种成分的含量

目的采用HPLC-MS/MS法同时测定脑血疏口服液中3种有效成分-芍药苷、黄芪甲苷及丹皮酚的含量。方法选用Phenomenex Luna C_(18)(100 mm×4.6 mm,5μm)色谱柱;以含10 mmol/mL乙酸铵乙腈溶液(A)、10 mmol/mL乙酸铵水溶液(B)为流动相,梯度洗脱;质谱为ESI源负离子-MRM模式下检测,流速为0.3mL/min;柱温为25℃。结果芍药苷、黄芩甲苷及丹皮酚3种成分线性范围分别为0.20~2.00μg(r=0.9991)、2.00~20.00μg(r=0.999 0)、1.00~10.00μg(r=0.998 5),3种化合物的平均回收率分别为100.1%、97.9%、102.3%。结论本方法简便、快捷,重现性好,适用于同时测定脑血疏口服液中芍药苷、黄芪甲苷及丹皮酚的含量。     

HPLC法同时测定桂枝茯苓胶囊中丹皮酚、芍药苷和苦杏仁苷的含量

目的：建立HPLC法同时测定桂枝茯苓胶囊中丹皮酚、芍药苷和苦杏仁苷的含量。方法：采用HPLC法测定桂枝茯苓胶囊中丹皮酚、芍药苷和苦杏仁苷的含量。采用C18柱,流动相为甲醇∶水（55∶45）洗脱,流速为1.0ml·min-1,检测波长为274nm,柱温为30℃,进样体积为10μL。结果：线性范围分别为0.198～3.166μg（r=0.9998）、0.195～3.128μg（r=0.9996）、0.197～30158（r=0.9997）。平均加样回收率分别为99.81%（RSD=2.48%）、99.69%（RSD=1.47%）、99.79%（RSD=2.12%）。结论：本研究建立的方法简便,结果稳定可靠,可用于桂枝茯苓胶囊的质量控制。     

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.