稳心律合剂指纹图谱的建立及共有峰的液质联用分析

目的建立稳心律合剂的指纹图谱,对共有峰进行质谱识别鉴定,为稳心律合剂质量标准的建立提供参考。方法根据稳心律合剂的制剂工艺制备10批次制剂并进行液质联用检测分析。流动相为乙腈(A)-0.1 mL·L~(-1)甲酸水溶液(B):0～10 min,5%A～20%A;10～15 min,20%A～23%A;15～30 min,32%A～68%A;30～40 min,32%A;40～50 min,32%A～38%A;50～60 min,38%A～48%A;60～70 min,48%A～65%A。柱温:30℃;流速:0.4 mL·min~(-1);检测波长:254 nm;进样量:10μL。结果 10批稳心律合剂特征图谱中有26个共有峰,其相似度均大于0.985。结论该研究建立的指纹图谱相似度高,共有峰中识别鉴定的9个特征峰可适用于稳心律合剂的质量标准制定研究。     

山枝仁药材指纹图谱研究

目的:建立川产山枝仁药材的指纹图谱,为山枝仁药材的质量控制提供依据。方法:采用HPLC法进行山枝仁成分分析,色谱柱为Diamonsil C_(18)柱(250 mm×4.6 mm,5μm);流动相A∶0.4%磷酸水;B:甲醇,流动相梯度洗脱:0~10 min,10%~40%B;10~25 min,40%~55%B;25~30 min,60%~90%B;30~42 min,60%~90%B;42~43 min,90%~95%B;43~60 min,95%~95%B;流速1 mL·min~(-1);检测波长360 nm;柱温30℃;进样量10μL。通过指纹相识度评价软件对指纹图谱进行评价。结果:建立了山枝仁的指纹图谱,13个共有峰,10批样品与共有峰指纹图谱相似度均在0.90以上。符合指纹图谱相关要求。结论:本方法简便、快捷、可靠,为提高山枝仁药材质量控制标准提供参考。     

进口药材司卡摩尼亚脂质量标准提高研究

目的:提高进口药材司卡摩尼亚脂的质量标准。方法:收集23批司卡摩尼亚脂药材,按照《中华人民共和国药典》方法进行系统的水分、总灰分、酸不溶性灰分、浸出物、重金属及有害元素和农药残留分析测定;分别采用UV、TLC进行定性鉴别研究;采用HPLC特征图谱研究,色谱柱为Agilent ODS-AQ(4.6 mm×150 mm, 5μm),流动相为甲醇(A)-0.4%磷酸水溶液(B),梯度洗脱(0～5 min, 30%A;5～10 min, 30%A→40%A;10～15 min, 40%A;15～20 min, 40%A→55%A;20～30 min, 55%A→70%A;30～32 min, 70%A→95%A;32～45 min, 90%A;45～55 min, 100%A;55～60 min, 100%A→30%A;60～70 min, 30%A),流速为1.0 mL·min^-1,检测波长为254 nm,柱温为35℃。建立HPLC指纹图谱,以4号峰为参照,采用《中药色谱指纹图谱相似度评价系统(2012版)》进行相似度评价。结果:司卡摩尼亚脂药材的性状鉴别专属;UV光谱...     

儿童清咽解热口服液高效液相色谱指纹图谱研究

目的建立儿童清咽解热口服液的指纹图谱,为制剂的质量控制提供参考依据。方法采用HPLC法,色谱柱为Phenomenex Gemini-C18(250 mm×4.6 mm,5μm);流动相A为乙腈,流动相B为0.2%磷酸溶液,梯度洗脱(0～15 min,3%～17%A;15～35 min,17%～28%A;35～50 min,28%A;50～65 min,28%～65%A;65～70 min,65%～95%A;70～80 min,95%A);柱温35℃;流速1.2 mL·min~(-1);检测波长206 nm;进样量10μL。结果 12批儿童清咽解热口服液的相似度较好,均在0.98以上,得到了12个共有峰,指认了秦皮乙素、黄芩苷、甜菊素3种成分。结论本研究建立了儿童清咽解热口服液的指纹图谱,此方法简便可靠,重现性好,可为制剂的质量控制提供参考。     

白芍饮片的HPLC指纹图谱建立及聚类分析、主成分分析

目的:建立白芍饮片的高效液相色谱(HPLC)指纹图谱,并进行聚类分析和主成分分析。方法:采用HPLC法。色谱柱为SunFire~?C18,流动相为乙腈-0.05%磷酸水溶液(梯度洗脱),流速为1.0 mL/min,检测波长为230 nm,柱温为30℃,采集时间为70min,进样量为15μL。以芍药苷为参照,建立26批不同产地白芍饮片及30批不同炮制方法白芍饮片的HPLC指纹图谱;采用《中药色谱指纹图谱相似度评价系统》(2012版)进行相似度评价,确定共有峰;采用SPSS 20.0软件进行聚类分析和主成分分析。结果:26批不同产地白芍饮片共有9个共有峰,相似度均大于0.880;共指认了6个峰,分别为没食子酸、儿茶素、芍药内酯苷、芍药苷、1,2,3,4,6-五没食子酰葡萄糖、苯甲酰芍药苷;聚类分析结果显示,当余弦距离为15时26批样品可聚为2类,S1～S21聚为一类,S22～S26聚为一类;经主成分分析,前2个主成分的累积方差贡献率为81.124%。30批不同炮制方法白芍饮片共有10个共有峰,相似度均大于0.970;共指认了7个峰,分别为没食子酸、儿茶素、丹皮酚新苷、芍药内酯苷、芍药苷、1,2,3,4,6-五没食子酰葡萄糖、苯甲酰芍药苷;聚类分析结果显示,当余弦距离为25时,30批样品可聚为2类,B1～B10聚为一类,C1～C10、J1～J10聚为一类;经主成分分析,前4个主成分的累积方差贡献率为86.887%。结论:所建HPLC指纹图谱及聚类分析和主成分分析结果可为不同白芍饮片的质量控制提供参考。     

朱砂安神丸高效液相色谱数字化指纹图谱研究

目的建立朱砂安神丸(Zhusha Anshen Wan,ZSASW)HPLC数字化指纹图谱,作为其整体质量控制的一个判据标准。方法采用反相HPLC法,使用Century SIL C18BDS柱(200 mm×4.6 mm,5μm),以0.2%H3PO4溶液(A)-0.1%H3PO4乙腈溶液(B)为流动相进行梯度洗脱(0~10 min,0→15%B;10~30 min,15%→30%B;30~50 min,30%→70%B;50~60 min,70%→85%B),流速1.0 mL.min-1,检测波长203 nm,柱温(30±0.15)℃,进样量5μL。以色谱指纹图分离量指数(chromatographic fingerprint resolution index,RF)为目标函数优化试验条件,用"中药色谱指纹图谱超信息特征数字化评价系统3.0"软件进行数字化评价。结果以盐酸小檗碱(berberine hydrochloride,BBR)为参照物峰,确定57个共有指纹峰,获得判别其质量的重要数字化信息,以系统指纹定量法鉴别出S1、S2、S3、S4、S9和S12质量极好,S5、S6和S10质量很好,S11质量好,S7和S8质量为劣。结论所建立的ZSASW-HPLC数字化指纹图谱可清晰反映ZSASW的局部和整体指纹的质量变异,用数字化指纹图谱控制中药质量准确可行。     

五加生化胶囊UPLC-MS指纹图谱研究

目的:建立五加生化胶囊UPLC-MS的指纹图谱,为科学客观地评价其质量提供可靠的方法。方法:色谱柱:ACQUITYUPLC BEH(2.1mm×50 mm,1.7μm);流动相:乙腈(A)-0.1%甲酸和10 mmol.L-1醋酸铵(B)梯度洗脱[5.0%A(0 min),5.0%A→50%A(0～10 min),50%A～80%A(10～16 min)];柱温:40℃;流速:0.4 mL.min-1;进样量:8μL;电喷雾接口,正离子模式,毛细管电压3.50 kV,锥孔电压35.00 V,离子源温度120℃,脱溶剂温度380℃,脱溶剂气N2:500 L.h-1,锥孔气N2:50 L.h-1。结果:11批五加生化胶囊UPLC-MS指纹图谱中共标定了37个共有色谱峰,通过与对照品的保留时间及质谱信息的比对,确定4号、8号、9号、10号和30号峰分别为紫丁香苷、阿魏酸、甘草苷、异嗪皮啶和藁本内酯。结论:所建立的五加生化胶囊UPLC-MS指纹图谱满足于方法学的要求,所得的指纹图谱特征性及专属性强,可用于五加生化胶囊质量的控制。     

HPLC指纹图谱结合正交试验优化红参的炮制工艺

目的:建立红参的高效液相色谱(HPLC)指纹图谱,并优选其最优炮制工艺。方法:采用HPLC法。色谱柱为Waters SymmetryShieldTMRP18,流动相为乙腈-水(梯度洗脱),柱温为30℃,流速为1.0 mL/min,检测波长为203 nm,进样量为10μL。以人参皂苷Rb1为参照,绘制10批红参样品的HPLC指纹图谱;采用《中药色谱指纹图谱相似度评价系统(2012A版)》进行相似度评价,并确定共有峰。以蒸制温度、蒸制时间、干燥方法为考察因素,人皂苷类成分含量、指纹图谱相似度为指标,采用L16(43)正交试验优化红参的炮制工艺并进行验证;采用SPSS 19.0软件对10批红参样品和最优工艺炮制品进行聚类分析。结果:10批红参共有13个共有峰,相似度均大于0.920;共指认人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1等3个共有峰。最优炮制工艺为100℃蒸制150 min,60℃干燥;验证试验结果显示,3批红参最优工艺炮制品中人参皂苷Rg1、Re、Rb1的含量分别为0.26%~0.29%、0.17%~0.20%、0.47%~0.54%,其指纹图谱与对照图谱相似度均大于0.970。聚类分析结果显示,10批红参及3批最优工艺炮制品可聚为两类,即HS3~HS10聚为一类、3批最优工艺炮制品及HS1、HS2聚为一类。结论:所建指纹图谱可用于红参的炮制工艺优化,能表征炮制工艺参数波动与药材整体质量的相关性变化;所得最优炮制工艺合理可行。     

香薷HPLC指纹图谱及多指标成分定量分析

目的:建立香薷的HPLC指纹图谱及其咖啡酸、迷迭香酸、木犀草素、芹菜素、黄芩素-7-甲醚、香荆芥酚、麝香草酚7个成分的HPLC含量测定方法。方法:采用Eclipse XDB-C₁₈色谱柱(250 mm×4.6 mm, 5μm),流动相为0.1%甲酸水溶液(A)-乙腈(B),梯度洗脱(0～17 min, 12%B→20%B;17～30 min, 20%B→30%B;30～40 min, 30%B→45%B;40～55 min, 45%B→54%B),流速为1.0 mL·min^-1,检测波长为280、330 nm,柱温为30℃,进样量为5μL。结果:建立了香薷HPLC指纹图谱，共确定了14个共有峰，并指认其中5个共有峰，分别为咖啡酸(5号峰)、迷迭香酸(10号峰)、黄芩素-7-甲醚(12号峰)、香荆芥酚(13号峰)、麝香草酚(14号峰),17批香薷样品的相似度均>0.910;对17批药材中指认的7个成分进行含量测定，其质量浓度分别在1.04～52.0μg·mL^-1(r=0.999 3,n=5)、6.0～300.0μg·...     

基于指纹图谱及化学模式识别方法优选蜜枇杷叶药材产地

目的:基于高效液相色谱指纹图谱和化学模式识别方法,评价不同产地蜜枇杷叶的质量,优选出蜜枇杷叶的最佳产地。方法:采用Acclaim^TM 120A C₁₈(250 mm×4.6 mm, 5μm)色谱柱进行检测,流动相为0.2%磷酸水溶液(A)-乙腈(B),梯度洗脱(0～5 min, 5%B;5～6 min, 5%B→10%B;6～20 min, 10%B;20～50 min, 10%B→25%B;50～60 min, 25%B),体积流量1.0 mL·min^-1,检测波长327 nm,柱温30℃,进样量10μL。建立30批不同产地蜜枇杷叶的指纹图谱,采用指纹图谱结合化学模式识别的方法对不同产地蜜枇杷叶进行综合分析,对不同产地蜜枇杷叶进行聚类分析(cluster analysis.CA)、主成分分析(principal component analysis.PCA)及综合评分,采用正交偏最小二乘判别分析(orthogonal partial least squares-discriminant analysis, OPLS-D...     

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.