HPLC测定舒筋活血片中4-甲氧基水杨醛的含量

目的建立舒筋活血片质量标准定量指标。方法采用HPLC测定舒筋活血片中4-甲氧基水杨醛的含量;色谱柱:Aichrom Reliasil C18柱(5μm,250 mm×4.6 mm);流动相:甲醇-水-四氢呋喃(50∶50∶0.2);流速:1.0 ml/min;柱温:35℃;检测波长:279 nm;理论塔板数按4-甲氧基水杨醛峰计算不低于3000。结果4-甲氧基水杨醛线性范围为0.06~0.55μg/μl(r=0.9992),平均加样回收率96.8%(n=6),RSD=0.99%。结论该方法操作简单,舒筋活血片的质量控制。     

HPLC测定舒筋活血片中4-甲氧基水杨醛的含量

目的 建立舒筋活血片质量标准定量指标.方法 采用HPLC测定舒筋活血片中4-甲氧基水杨醛的含量;色谱柱:Aichrom Reliasil C18柱(5 μm, 250 mm×4.6 mm);流动相:甲醇-水-四氢呋喃(50∶50∶0.2);流速:1.0 ml/min;柱温:35 ℃;检测波长:279 nm;理论塔板数按4-甲氧基水杨醛峰计算不低于3000.结果 4-甲氧基水杨醛线性范围为0.06～0.55 μg/μl(r=0.9992),平均加样回收率96.8%(n=6),RSD=0.99%.结论 该方法操作简单,舒筋活血片的质量控制.     

高效液相色谱法测定舒筋活血分散片中4-甲氧基水杨醛含量

目的建立舒筋活血分散片的含量测定方法。方法采用高效液相色谱法,对舒筋活血分散片中4-甲氧基水杨醛进行含量测定。色谱柱为Aichrom Reliasil C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-水-四氢呋喃(50∶50∶0.2),流速1.0 mL/min,柱温室温。结果 4-甲氧基水杨醛进样量在0.071 6～0.644 4μg范围内与峰面积线性关系良好(r=0.999 2);平均加样回收率为95.03%,RSD=3.17%(n=6)。结论该方法操作简便,结果稳定、可靠,可用于制剂的质量控制。     

舒筋活血片HPLC指纹图谱及多指标含量测定研究

摘要：目的:建立舒筋活血片的HPLC指纹图谱及多指标成分测定方法。方法:采用HPLC法,以Agilent ZORBAX Eclipse XDB-C18柱（250 mm×4.6 mm,5μm）为色谱柱,以甲醇（A）-0.1%磷酸水溶液（B）为流动相,梯度洗脱,流速为0.8 ml·min-1,检测波长为285 nm,柱温为30℃,进样量为20μl。以4-甲氧基水杨醛为参照,绘制13批样品的HPLC指纹图谱;采用《中药色谱指纹图谱相似度评价系统》（2004年A版）进行相似度评价,确定共有峰;采用SPSS 22.0软件对13批样品进行聚类分析,同时测定原儿茶酸、原儿茶醛、紫丁香苷、绿原酸、羟基红花黄色素A、芦丁、4-甲氧基水杨醛、α-香附酮、山柰素9种成分的含量。结果:13批舒筋活血片指纹图谱标定了共有峰24个,指认了其中9个化学成分。原儿茶酸、原儿茶醛、紫丁香苷、绿原酸、羟基红花黄色素A、芦丁、4-甲氧基水杨醛、α-香附酮、山柰素9种成分线性关系良好（r=0.999 2～0.999 8）,平均回收率在97.8%～100.8%之间。结论:所建立的HPLC指纹图谱及多指标成分测定可为舒筋活血片的质量评价提供参考。     

香加皮中4-甲氧基水杨醛含量测定方法的改进

目的改进香加皮中4-甲氧基水杨醛的含量测定方法。方法高效液相色谱法,色谱柱C18(250mm×4.6mm,5μm),流动相为甲醇-水-醋酸(70∶30∶2),流速为1.0mL·min-1,检测波长278nm。结果4-甲氧基水杨醛线性范围为4~32mg·L-1,r=0.9989(n=5),平均回收率为99.2%,RSD为1.1%。结论该法较原方法简便、准确,重复性好。     

HPLC切换波长法测定舒筋活血片中山奈素、4 甲氧基水杨醛和α 香附酮的含量

摘 要 目的：建立高效液相色谱法同时测定舒筋活血片中山奈素、4 甲氧基水杨醛、α 香附酮3成分的含量。方法: 采用BDS HYPERSIL C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以乙腈 1%冰乙酸为流动相,梯度洗脱,流速:1 ml·min^-1,检测波长:360 nm(0~7 min,测定山奈素)、278 nm（7~10 min,测定4 甲氧基水杨醛）、254 nm（10~30 min,测定α 香附酮）。 结果: 各待测成分分离度良好,山奈素、4 甲氧基水杨醛、α 香附酮的进样量分别在7.42~148.48 ng(r=0.999 8)、14.83~296.64 ng(r=0.999 9)、24.93~498.56ng(r=0.999 7)范围内与峰面积呈良好的线性关系;加样回收率分别为99.5%（RSD=1.3%）、98.9%（RSD=1.0%）、98.9%（RSD=1.4%）（n=6）。 结论:本方法简单、快速、灵敏、准确,可用于舒经活血片中山奈素、4 甲氧基水杨醛和α 香附酮的含量测定。     

HPLC法同时测定苦木注射液中3种活性成分的含量

目的:建立同时测定苦木注射液中3种活性成分3-甲基-铁屎米-2,6-二酮、4-甲氧基-5-羟基铁屎米酮、4,5-二甲氧基-铁屎米酮含量的分析方法。方法:采用高效液相色谱法,色谱柱为Phenom enex Gem in i C18(150 mm×4.6 mm,5μm)柱,流动相为pH 7.5的0.2 mol.L-1磷酸氢二钠及磷酸二氢钠缓冲液(A)?甲醇(B),梯度洗脱,流速1 mL.m in-1,检测波长254 nm,柱温30℃。结果:苦木注射液中3-甲基-铁屎米-2,6-二酮、4-甲氧基-5-羟基铁屎米酮、4,5-二甲氧基-铁屎米酮线性范围分别为0.0380~0.7600μg(r=0.9999),0.0450~0.9000μg(r=0.9999),0.0287~0.574μg(r=0.9999);平均加样回收率(n=9)分别为99.3%,101.4%,101.8%。结论:该方法操作简单,重复性好,为评价和监控苦木注射液的质量提供可靠的方法。     

舒筋活血胶囊质量标准研究

目的建立舒筋活血胶囊的质量标准。方法采用薄层色谱法（TLC）对制剂中的香附、红花和香加皮进行鉴别,采用高效液相色谱法（HPLC）测定制剂中4-甲氧基水杨醛的含量。结果TLC能较好地鉴别制剂中的香附、红花和香加皮;HPLC法能准确测定出制剂中4-甲氧基水杨醛的含量,其在2-751μg／ml范围之间呈良好的线性关系,平均回收率为96．6％（RSD=0．78％）。结论所建立的方法简单可行,能快速准确地对舒筋活血胶囊进行鉴别和含量测定。     

高效液相色谱法测定陈皮多甲氧基黄酮部位中3种黄酮的含量

目的:建立陈皮多甲氧基黄酮部位中3,5,6,7,8,3′,4′-七甲氧基黄酮、川陈皮素和 Natusdaidai 的高效液相色谱含量测定方法,并测定检测波长下各成分的响应因子,建立以3,5,6,7,8,3′,4′-七甲氧基黄酮为单指标测定3种多甲氧基黄酮总含量的方法。方法:采用 Kromasil C_(18)(4.6 mm×250 mm,5μm)色谱柱,流动相为乙腈-0.2%醋酸溶液(1:1);流速为1 mL·min~(-1),柱温为25℃,检测波长347 nm。结果:3,5,6,7,8,3′,4′-七甲氧基黄酮、川陈皮素、Natusdaidai 的线性范围分别为0.0732～0.732,0.0654～0.654,0.07～0.700μg,相关系数均为0.9999。加样回收率(n=5)分别为97.80%,96.71%,98.52%;RSD 分别为1.9%,1.2%,2.1%。3,5,6,7,8,3′,4′-七甲氧基黄酮、川陈皮素和 Natusdaidai 的响应因子(RF 值)分别为3283.6,3331.8,2503.4。结论:该方法简便、准确,可用于陈皮多甲氧基黄酮部位中3,5,6,7,8,3′,4′-七甲氧基黄酮等3种成分的含量测定。     

HPLC法同时测定通脉方中6个异黄酮类成分的含量

目的:建立HPLC-DAD法同时测定通脉方中3'-羟基葛根素、葛根素、3'-甲氧基葛根素、葛根素芹菜糖苷、大豆苷和大豆苷元6个异黄酮类有效成分的含量。方法:采用Dikma DiamonsilTM C18色谱柱(250 mm×4.6 mm,5μm),Dikma EasyGuardC18保护柱(20 mm×4.6 mm,5μm);以0.5%醋酸乙腈-0.5%醋酸水溶液为流动相,梯度洗脱,流速1.0 mL.min-1,检测波长250 nm,柱温为25℃。结果:6个异黄酮类成分的线性范围分别为:3'-羟基葛根素,6.25～200μg.mL-1(r=0.9998);葛根素,31.25～1000μg.mL-1(r=0.9996);3'-甲氧基葛根素,6.25～200μg.mL-1(r=0.9999);葛根素芹菜糖苷,6.25～200μg.mL-1(r=0.9998);大豆苷,6.25～200μg.mL-1(r=0.9995);大豆苷元,1.25～40μg.mL-1(r=0.9997)。平均加样回收率均在95.43%～103.9%,RSD均在0.40%～4.3%。结论:该方法准确,灵敏度高,重复性好,可用于通脉方中6个主要...     

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.