HPLC法同时测定蛇床子中蛇床子素和欧前胡素含量

目的用高效液相色谱法同时测定中药蛇床子中蛇床子素和欧前胡素的含量。方法采用KromasilC8(2 5 0mm× 4 6mm ,5 μm)为色谱柱 ,以甲醇 水 (体积比 6 5∶35 )为流动相的HPLC法 ,检测波长为 310nm ,流速为 0 8mL·min-1,柱温为室温。结果以醋酸氟轻松为内标 ,蛇床子素和欧前胡素分别在 13～ 2 0 8mg·L-1和 8～ 12 8mg·L-1内 ,线性关系良好 (r≥ 0 9998) ;平均回收率分别为 98 2 %和 97 5 % ;RSD分别为 1 7%和 2 0 % (n =9)。结论本法简便快速 ,回收率及重现性良好 ,适用于中药蛇床子中蛇床子素和欧前胡素的定量分析     

HPLC法测定复方沙棘籽油栓中蛇床子素的含量

目的测定复方沙棘籽油栓中主要成分蛇床子素的含量。方法采用HPLC法,C8色谱柱;流动相为甲醇-水(75∶25);流速0.7 mL.min-1;检测波长320 nm;柱温30℃;进样量为10μL。结果蛇床子素含量与峰面积线性关系良好,回归方程为A×10-3=-7.950+7.384 X,r=0.999 5(n=5),平均回收率为98.3%,RSD值为0.71%。结论HPLC法测定复方沙棘籽油栓中蛇床子素的含量可行。     

HPLC测定寄生追风液中独活的有效成分蛇床子素

目的 :建立寄生追风液中蛇床子素的 HPL C含量测定方法。方法 :采用乙醚提取样品 ,Synchrom ODS柱 (5μm,15 0 mm× 4.6 m m)。流动相为甲醇 - 0 .1m ol· L- 1硫酸铵溶液 (70∶ 30 ) ,用硫酸溶液 (1→ 5 )调节 p H为 2 .5。检测波长 32 2 nm。结果 :线性范围 0 .0 34～ 0 .2 7μg(r=0 .99995 ) ,平均回收率 98.0 8% (n=6 )。结论 :用于寄生追风液质量控制     

HPLC测定生泰胶囊中蛇床子的含量

目的　测定生泰胶囊中蛇床子素的含量。方法　采用HPLC法 ,色谱柱ShimpackCLC -ODS(15 0mm× 4 .6mm ,5 μm) ;甲醇 -水 -四氢呋喃 (70∶4 0∶5 )为流动相 ;检测波长 317nm ;柱温 35℃。结果　在 0 0 5 12 5～ 1 14 8μg线性范围 (r=0 .9990 ) ,平均加样回收率 97 2 % ,RSD =1.16 % (n =3) ,3批样品平均含量为每粒 2 72mg。结论　该法分离效果好 ,灵敏度高且准确。     

舒洁洗液质量标准研究

目的 建立舒洁洗液的质量标准.方法 以蛇床子素为对照品,苯-乙酸乙酯(30:1)为展开剂对其中蛇床子药材进行薄层色谱鉴别;以苦参碱为对照品,三氯甲烷-甲醇-氨水(15:4:0.5)为展开剩对其中苦参药材进行薄层色谱鉴别;采用反相高效液相色谱法测定主药蛇床子中蛇床子素含量.结果 薄层色谱斑点清晰,重现性好,阴性对照无干扰;高效液相色谱理论塔板数以蛇床子素峰计为4 750.线性范围为0.1～0.5μg,r=0.999 9(n=5),平均回收率为99.64%,RSD:0.51%(n=6).结论 方法简便准确,重现性好,可用于该制剂的质量控制.     

RP-HPLC法测定抗妇炎泡腾栓中蛇床子素和盐酸小檗碱的含量

目的:建立以反相高效液相色谱法测定抗妇炎泡腾栓中蛇床子素和盐酸小檗碱含量的方法。方法:色谱柱为Diamonsil C18(250mm×4·6mm,5μm),流动相为乙腈-0·2%磷酸溶液(52∶48,每100mL含0·1g十二烷基磺酸钠),检测波长为322nm,流速为1mL·min-1,柱温为30℃。结果:蛇床子素、盐酸小檗碱进样量分别在0·0198~0·3960μg(r=0·99997)、0·05665~1·13300μg(r=0·99999)范围内与各自峰面积积分值呈良好线性关系;平均加样回收率分别为101·06%(RSD=1·10%)、101·88%(RSD=0·98%)。结论:本方法简便、准确、重现性好,可用于抗妇炎泡腾栓的质量控制。     

HPLC法同时测定追风舒经活血片中4种成分的含量

目的:建立同时测定追风舒经活血片中羌活醇、异欧前胡素、蛇床子素和二氢欧山芹醇当归酸酯含量的方法。方法:采用高效液相色谱法。色谱柱为Hypersil C18(200 mm×4.6 mm,5μm),流动相为乙腈-0.05%冰醋酸溶液(梯度洗脱),流速为0.8 ml/min,检测波长为310 nm(羌活醇和异欧前胡素)、330 nm(蛇床子素和二氢欧山芹醇当归酸酯)。结果:羌活醇、异欧前胡素、蛇床子素和二氢欧山芹醇当归酸酯的线性范围分别为0.027 8⁰.556 0μg(r=0.999 5)、0.018 40.556 0μg(r=0.999 5)、0.018 4⁰.368 0μg(r=0.999 4)、0.059 20.368 0μg(r=0.999 4)、0.059 2¹.184 0μg(r=0.999 8)、0.012 61.184 0μg(r=0.999 8)、0.012 6⁰.252 0μg(r=0.999 3);四者精密度、稳定性、重复性试验的RSD<1%;平均加样回收率分别为98.69%(RSD=0.86%,n=6)、96.92%(RSD=0.62%,n=6)、99.13%(RSD=0.95%,n=6)、97.79%(RSD=1.38%,n=6)。结论:该方法准确、灵敏、重复性好,可用于追风舒经活血片的质量控制。     

改变检测波长HPLC法测定红霉素的含量

采用改变检测波长法 ,以 C18为固定相 ,以乙腈 -甲醇 - 0 .2 mol/L醋酸铵溶液 -水 ( 4 5∶ 1 0∶ 1 0∶ 35 ,p H=6.8)为流动相测定红霉素的含量。检测波长 :0～ 5 min(基线 )为 32 0 nm,5～ 8min(色谱峰 )为 2 1 5 nm。红霉素浓度在 0 .45～ 2 .7mg/ml范围内与峰面积呈良好的线性关系 ,回归方程为 Y× 1 0 -4 =0 .0 2 3+ 1 .2 38X,r =0 .9997,平均回收率 97.1 %     

高效液相色谱法测定滴霉洗剂中蛇床子素的含量

目的研究滴霉洗剂中蛇床子素含量测定的方法。方法采用高效液相色谱法以甲醇 水 (75∶2 5 )为流动相 ,色谱柱为AlltimaC18(2 5 0mm× 4.6mm ,5 μm) ;流速为 1ml/min ;检测波长为 32 2nm。结果线性范围为 6 .0～18.0 μg ,r =0 .9999,加样回收率为 98.99% ,RSD为 0 .86 % (n =6 )。结论此法简便易行 ,结果准确 ,重现性好 ,灵敏度高 ,可用于控制生药及制剂的质量     

正交设计法优选白芷的提取工艺

目的以欧前胡素、异欧前胡素的提取总量为考察指标,对影响香豆素类化合物提取工艺的因素进行研究,优选白芷的最佳提取工艺。方法采用RP HPLC法,AccusilC18柱( 2 5 0mm×4 6mm ,10 μm) ,流动相为甲醇 水(体积比6 5∶35 ) ;检测波长2 5 1nm。结果欧前胡素与异欧前胡素分别在0 76 8～19 2 0mg·L-1(r =0 9997)、0 2～16 0mg·L-1(r =0 9998)内与峰面积呈良好的线性关系(n =6 ) ,方法回收率(n =9)分别为96 8%、98 0 % ,RSD分别为2 0 %、1 9%。结论白芷的最佳提取工艺为A3 B2 C3 ,即用8倍量的95 % (w)的乙醇提取3次,每次4h。     

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.     

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.     

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.     

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.