HPLC测定熊胆降热丸中的儿茶素

目的 建市测定熊胆降热丸中儿茶素含量的方法.方法 采用Luna C_(18)色谱柱(150 mm×4.6 mm,5μm),流动相为乙腈-水(8:92),流速为1.0 mL·min~(-1),检测波长为280 nm,柱温为35℃.结果 儿茶素9.62～231.00μg·mL~(-1)与峰而积的线性关系良好(r=0.9996),平均回收率为95.88%,重复性试验的RSD=0.63%(n=6).结论 所建方法简便、快速、准确,适用于熊胆降热丸的质量控制.     

HPLC法测定肾康丸中大黄酚、大黄素的含量

目的:建立肾康丸中大黄酚、大黄素的含量测定方法。方法:采用HPLC法,色谱柱为Diamonsi C18(250 mm×4.6 mm,5μm),流动相为乙腈-甲醇-0.1%磷酸溶液(42∶23∶35),流速为1.0 ml.min-1,检测波长为254 nm,进样量10μl。结果:大黄酚在9.38～150.00μg.ml-1(r=1.000 0),大黄素在3.31～53.00μg.ml-1(r=1.000 0)之间线性关系良好,其平均加样回收率大黄酚为99.83%,RSD为0.75%;大黄素为99.73%,RSD为0.34%。结论:此法简便,结果准确、灵敏,可用于肾康丸的含量测定。     

高效液相色谱法同时测定九制大黄丸中5组分含量

目的 建立同时测定九制大黄丸中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚含量的高效液相色谱(HPLC)法。方法 色谱柱为C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸溶液(77∶23),流速1.0 m L/min,检测波长254 nm,柱温40℃,进样量20μL。结果 芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的进样质量浓度线性范围分别为4.6~92μg/m L,3.8~76μg/m L,4.0~800μg/m L,5.0~100μg/m L和17.6~352μg/m L,平均回收率分别为99.38%,99.04%,99.72%,99.59%和99.52%,RSD分别为0.80%,1.02%,0.50%,0.54%,0.92%(n=6)。结论 HPLC法可同时测定九制大黄丸中5组分的含量,专属性强,分离效果好。     

乌金止痛丸中大黄的质量标准

目的建立乌金止痛丸中大黄素和大黄酚的高效液相色谱法测定方法。方法采用Shimadzu LC-10A高效液相色谱仪,以ShimadzuC18(4.6mm×250mm,5μm)为色谱柱;流动相为磷酸-0.1%磷酸溶液(75∶25);流速1.0mL.min-1,检测波长254nm。结果大黄素在0.01803~0.9016μg(r=0.99992)、大黄酚在0.01198~0.5992μg(r=0.99993)范围内呈良好线性关系;样品平均回收率:大黄素98.04%,RSD为0.75%;大黄酚97.74%,RSD为0.62%。结论大黄素和大黄酚的HPLC方法精密度、重现性和分离效果好,分析快速,适合于乌金止痛丸中大黄的质量控制。     

HPLC-MS法测定首乌丸中五种蒽醌类成分的含量

目的建立首乌丸中芦荟大黄素、大黄酸、大黄素、大黄酚以及大黄素甲醚等五种蒽醌类成分的含量测定方法。方法 HPLC-MS联用法对首乌丸中五种蒽醌类物质的含量同时测定。色谱条件为:Phenomenex Luna C18(3μm,150 mm×2 mm)柱,流动相:甲醇-5 mmol/L醋酸铵溶液(90∶10),流速:0.2 mL/min,电喷雾型质谱检测器。结果大黄酸、芦荟大黄素、大黄素、大黄酚、大黄素甲醚分别在0.18～56.6,0.016～10.03,0.024～14.94,0.18～11.33,0.011～6.85 ng范围内线性良好;r分别为0.999 8,0.999 9,0.998 8,0.999 9,0.999 9;水解前平均回收率分别为108.5%(RSD=0.93%),98.67%(RSD=1.57%),100.2%(RSD=0.69%),99.73%(RSD=1.27%),105.4%(RSD=1.54%);水解后平均回收率分别为99.67%(RSD=1.12%),99.21%(RSD=1.78%),98.94%(RSD=1.23%),98.32%(RSD=2.08%),96.10%(RSD=2.67%)。结论此法简便、准确、快捷,可用于首乌丸的质量控制。     

高效液相色谱法同时测定麻仁丸中大黄素、大黄酚、大黄酸、大黄素甲醚、芦荟大黄素的含量

目的建立麻仁丸中大黄素、大黄酚、大黄酸、大黄素甲醚、芦荟大黄素的含量测定方法。方法采用奥泰ALLTIMA-C18色谱柱(4.6 mm×250 mm,5μm),以甲醇(A)-0.1%磷酸溶液(B)为流动相,梯度洗脱[0~9min,60%A;9~20 min,60%→80%A;20~45 min,80%A];流速:1.0 mL.min-1;柱温:30℃;检测波长254 nm。结果大黄素、大黄酸、大黄酚、大黄素甲醚、芦荟大黄素线性范围分别为在9.08~81.72、8.4~75.6、13.42~120.7、7.56~68.04、8.2~73.8μg.mL-1,与峰面积线性关系良好,平均回收率分别为99.1%、99.6%、99.4%、99.8%、99.2%,RSD分别为2.0%、1.8、3.2%、1.1%、1.5%。结论本方法可作为麻仁丸中大黄素、大黄酚、大黄酸、大黄素甲醚、芦荟大黄素含量测定的一种准确、灵敏、可行的方法。     

反相高效液相色谱法测定清胃消滞丸中大黄素、大黄酚含量

目的:建立清胃消滞丸中大黄素和大黄酚含量的测定方法.方法:采用反相高效液相色谱法,以Hypersil C18柱(250 mm×4.6 mm,5μm)为流动相,流速为1 mL/min,检测波长为254 nm,柱温为25℃,以外标法检测.结果:大黄素浓度线性范围为3.06～30.60μg/mL(r=0.999 9),平均回收率为100.92%,RSD为1.28%(n=6);大黄酚浓度线性范围为6.13～61.30μg/mL(r=0.999 9),平均回收率为100.70%,RSD为1.20%(n=6).结论:该方法样品分离度佳、灵敏度高、重现性好,结果准确可靠.     

RP-HPLC测定热灼平喷雾剂中的大黄酸、大黄素和大黄酚

目的 采用RP-HPLC法测定热灼平喷雾剂中的大黄酸、大黄素、大黄酚.方法采用Luna-C18色谱柱(150mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸(80:20),柱温25°C,流速1.0 ml·min-1,检测波长254 nm.结果 大黄酸、大黄素、大黄酚的线性范围分别为85.2～852.0μg(r=0.9999)、88.0～880.0μg(r=0.9998)、107.2～1072.0μ g(r=0.9999),平均回收率分别为99.88%(RSD=3.02%)、105.0%(RSD=2.45%)、102.5%(RSD=1.48%).结论 所建方法简便、准确.     

用HPLC法测定牛黄上清片中各大黄素成分的含量

目的:建立HPLC同时测定牛黄上清片中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚含量的方法.方法:色谱柱为Shimadzu VP-ODS柱(4.6 mm×250 mm,5 mm),流动相为乙腈-0.1%磷酸梯度洗脱,流速为1.0 ml/min,检测波长为254 nm,柱温30℃.结果:芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚分别在0.042～0.840μg(r=0.9996)、0.168～3.352μg(r=0.9998)、0.084～1.680 μg(r=0.9997)、0.093～1.852μg(r=0.9999)和0.174～3.488μg(r=0.9994)内呈良好线性关系,平均回收率分别为99.8%(RSD=1.34%)、99.8%(RSD=1.72%)、100.0%(RSD=0.89%)、99.5%(RSD=0.97%)和100.2%(RSD=1.04%).结论:本方法简便、快速、准确,可用于牛黄上清片的质量控制.     

高效液相色谱法测定中药退黄外洗液中大黄酸、大黄素、大黄酚的含量

目的 建立中药退黄外洗液中大黄酸、大黄素、大黄酚的含量测定方法.方法 采用高效液相色谱(HPLC)法测定大黄酸、大黄素、大黄酚的含量,色谱柱:Phenomenex Gemini 5μm C18 110A 4.6×250.0mm 5micron;流动相:甲醇-0.1%磷酸溶液(85:15),流速:1.0ml/min,检测波长:254nm,柱温:35℃.结果 大黄酸在1.6576～33.1520μg/ml、大黄素在1.4976～29.9520μg/ml、大黄酚在1.7040～34.0800μg/ml范围内线性关系良好(r=1).大黄酸平均回收率为99.07%,RSD为0.85%(n=5);大黄素为99.14%,RSD为1.08%(n=5);大黄酚为99.94%,RSD为0.77%(n=5);阴性对照无干扰.结论 该方法操作简便、稳定、专属性强,可作为该制剂的质量控制方法.     

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.