HPLC法测定野菊花注射液中绿原酸的含量

目的建立野菊花注射液中绿原酸的含量测定方法。方法用HPLC法,分析色谱柱为ODS(150mm×4.6mm,5μm),流动相为甲醇-0.1mol/L磷酸二氢钠溶液(23:77)为流动相;检测波长327nm。结果精密度试验(n=6)RSD为0.55%,重现性实验(n=6)RSD为2.12%;平均回收率(n=6)为:92.23%,RSD=1.54%。三批野菊花注射液中绿原酸的含量为175.02￣188.58μg.ml-1。结论该法简单,可靠,可用来测定野菊花注射液中绿原酸的含量。     

病毒合剂(Ⅱ)中黄芩苷、绿原酸和橙皮苷的含量测定

目的:建立HPLC法同时测定病毒合剂中黄芩苷、绿原酸和橙皮苷的含量。方法:色谱柱为Acclaim120 C18120A(150 mm×4.6 mm,5μm),流动相A为0.4%磷酸,流动相B为乙腈,梯度洗脱,流速1.0 ml/min,检测波长300 nm,进样量10μl。结果:黄芩苷、绿原酸和橙皮苷分别在29.16~121.50μg/ml(r=0.999 9)、3.23~13.44μg/ml(r=0.999 7)和6.55~27.30μg/ml(r=0.999 9)范围内与峰面积呈良好线性关系。平均回收率黄芩苷为102.6%(RSD为0.87%,n=6),绿原酸为100.1%(RSD为0.96%,n=6),橙皮苷为98.38%(RSD为0.38%,n=6)。结论:本方法简便、快速、结果准确、重现性好、灵敏度高,可用于病毒合剂的质量控制。     

高效液相色谱法测定强肝口服液中绿原酸含量

目的 建立测定强肝口服液中绿原酸含量的高效液相色谱(HPLC)法.方法 采用XBridgeTM C18色谱柱(150mm x4.6mm,5μm).流动相为甲醇-0.1%磷酸溶液(15:85),检测波长323 nm,柱温为室温,流速1.0 mL/min.结果绿原酸进样量在0.0258～0.4644μ范围内与峰面积线性关系良好(r=0.9998),平均加样回收率为97.66%,RSD=0.93%(n=6).结论该法简便、快速、灵敏、准确、专属、重现性好,为强肝口服液的绿原酸含量测定提供了可靠方法.     

高效液相色谱法测定妇科止痒胶囊中绿原酸含量

目的建立测定妇科止痒胶囊中绿原酸含量的高效液相色谱(HPLC)法。方法采用XBridgeTM-C18色谱柱(150 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸溶液(15∶85),流速1.0mL/min,检测波长332nm。结果绿原酸进样量在0.0258～0.4644μg范围内与峰面积积分值线性关系良好,回归方程Y=2588978X-20732.66(r=0.9998),平均加样回收率为98.36%,RSD为1.29%(n=6)。结论该法简便、准确、重复性好,为测定妇科止痒胶囊的绿原酸含量提供了可靠的分析方法。     

HPLC法同步测定金银花中绿原酸和咖啡酸含量

目的同步测定河南产金银花中绿原酸和咖啡酸的含量。方法采用RP-HPLC方法测定,采用Kromasil-C18(4.6mm×250mm,5μm)色谱柱进行分离,流动采用甲醇-水(含0.2%醋酸)系统梯度洗脱,流速1.0ml/min,检测波长为280nm,柱温为30℃,进样体积10μL。结果绿原酸、咖啡酸分别在下列范围内有良好的线性和回收率:0.980～9.800μg(r=0.9999),99.85%(n=6,RSD=2.0%);0.00432～0.432μg(r=0.9992),98.7%(n=6,RSD=1.8%)。结论同步测定金银花中有机酸含量更加有利于金银花药材的质量控制。     

HPLC法测定珍杞降糖胶囊中绿原酸的含量

目的建立珍杞降糖胶囊中绿原酸的HPLC含量测定方法。方法采用HPLC法,色谱柱为AgilengtEclipsePlusC18柱(4.6mm×100mm);流动相:乙腈-0.4%磷酸(17︰83);流速:0.6mL/min;检测波长:327nm。结果绿原酸在0.0433～0.6938μg范围内线性关系良好(r=0.9999),平均加样回收率为98.39%,RSD=0.58%(n=6)。结论本方法简便快速、结果准确,可较好地控制该制剂的质量。     

两种不同方法测定注射用阿魏酸钠的含量

目的比较注射用阿魏酸钠含量的两种不同测定方法。方法分别采用紫外分光光度(UV)法及高效液相色谱(HPLC)测定。UV法采用纯化水为溶剂,310nm为测定波长;HPLC法采用Wa-tersXTerraRP18(4.6mm×250mm,5μm)色谱柱,流动相为甲醇-水(62∶38),流速为1ml/min,检测波长为310nm。结果 UV法中阿魏酸钠在6.216～14.504μg/ml范围内,浓度与吸光度呈良好线性关系(r=0.9999),平均回收率99.71%,相对标准偏差(RSD)为0.92%。HPLC法中阿魏酸钠在44.08～220.4μg/min范围内线性关系良好(r=0.9997),平均回收率98.79%,相对标准偏差(RSD)为1.61%。结论两种方法含量测定结果无明显差异,均可作为注射用阿魏酸钠含量测定的方法,可将UV法用于制剂半成品含量控制,而将HPLC法用于成品的含量控制,可缩短检验时间,保证制剂质量。     

HPLC-DAD法同时测定肝八味胶囊中4种成分的含量

目的 用高效液相色谱(HPLC)法同时测定肝八味胶囊中4种成分的含量。方法 采用HPLC法,色谱柱为C18柱(250mm×4.6mm,5μm),以乙腈为流动相A,以水为流动相B,梯度洗脱;检测波长为240nm;流速1.0ml/min。结果 丹酚酸B对照品在15.026~100.17μg/ml范围内呈良好线性关系,平均加样回收率为96.6%(n=6),RSD=1.8%(n=6);芍药苷对照品在14.335~95.564μg/ml范围内呈良好线性关系,平均加样回收率为97.0%(n=6),RSD=1.7%(n=6);虎杖苷对照品在8.235~54.90μg/ml范围内呈良好线性关系,平均加样回收率为97.2%(n=6),RSD=1.8%(n=6);大黄素对照品在1.582 5~10.55μg/ml范围内呈良好线性关系,平均加样回收率为98.1%(n=6),RSD=1.7%(n=6)。结论 此法简单准确、重现性好、专属性强、阴性对照无干扰,适用于肝八味胶囊的质量控制。     

银翘解毒丸(大蜜丸)中绿原酸含量测定方法研究

目的探讨银翘解毒丸(大蜜丸)质量标准。采用HPLC法对银翘解毒丸(大蜜丸)中的绿原酸进行含量测定。方法色谱柱为Kromasil C18色谱柱(4.6×250mm,5μm),以乙腈-0.3%磷酸(10∶90)为流动相;流速:1.0mL.min-1,检测波长327nm。结果绿原酸的进样量在0.03～0.15mg范围内呈良好的线性关系(r=0.9995),平均加样回收率为100.6%,RSD为1.57%(n=6)。结论方法简便、准确,可用于银翘解毒丸(大蜜丸)中绿原酸的含量测定。     

毒热清颗粒的质量标准研究

目的为新制剂毒热清颗粒建立质量标准。方法对制剂中连翘、紫花地丁、甘草采用薄层色谱(TLC)法进行定性鉴别;采用高效液相色谱法(HPLC)测定毒热清颗粒中黄芩苷、绿原酸的含量。色谱柱为Agilent ZORBAX XDB-C18柱(4.6mm×150mm,5μm),流动相甲醇-0.4%磷酸(梯度洗脱),流速1.0m L/min,检测波长为316nm,柱温25℃。结果连翘、紫花地丁、甘草的TLC图斑点清晰,分离度好。黄芩苷、绿原酸检测进样量线性范围分别为0.4764~2.382μg(r=0.9999),0.4216~2.108μg(r=0.9999),加样回收率分别为98.8%(RSD=1.5%),99.1%(RSD=1.1%),精密度、重复性、稳定性实验的RSD2%,n均为6。结论所建质量控制方法科学合理,可作为毒热清颗粒的质量标准。     

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.     

Pharmacological treatment of COVID-19: an opinion paper

The precocity and efficacy of the vaccines developed so far against COVID-19 has been the most significant and saving advance against the pandemic. The development of vaccines has not prevented, during the whole period of the pandemic, the constant search for therapeutic medicines, both among existing drugs with different indications and in the development of new drugs. The Scientific Committee of the COVID-19 of the Illustrious College of Physicians of Madrid wanted to offer an early, simplified and critical approach to these new drugs, to new developments in immunotherapy and to what has been learned from the immune response modulators already known and which have proven effective against the virus, in order to help understand the current situation.     

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.