高效液相色谱法测定丙谷胺片的含量

目的 　建立高效液相色谱法 (外标法 )测定丙谷胺片的含量。 方法 　采用 Agilient Hypersil ODS柱 (4 .0 mm× 2 5 0 mm,5μm) ,检测波长2 2 5 nm,流动相为甲醇 -水 (60∶ 40 ) ,流速为 1.0 ml·min- 1 ,外标法。结果 　测得线性范围 :12 .3 6～ 12 3 .6μg·m L- 1 ,回收率 99.3 2± 0 .89% (n=6) ,RSD为 1.44 %。 结论 　该方法操作简便、结果准确、重现性好。     

小儿酚氨咖敏颗粒含量测定方法改进研究

提高小儿酚氨咖敏颗粒含量测定质量标准,更有效的控制其含量.用HPLC法同时测定氨基比林、对乙酰氨基酚和咖啡因的含量.采用Diamonsal C18色谱柱,流动相为乙腈-0.05mol·L-1磷酸二氢钾溶液-三乙胺-磷酸(10∶90∶0.02∶0.03)(调节pH值为3.5),流速为1ml·min-1,检测波长215nm.线性关系与回收率氨基比林0.06～1.80μg(r=0.9999),101.22%(RSD=0.45%);对乙酰氨基酚0.075～2.25μg(r=0.9999),101.27%(RSD=0.51%);咖啡因0.02～0.6μg(r=0.9999),100.7%(RSD=0.70%).方法简便,准确,重现性好.     

HPLC法测定复方丙谷胺片含量

目的：拟建立用高效液相色谱法测定复方丙谷胺片中丙谷胺含量的方法。方法：采用Diamonsil C18色谱柱（250 mm×4.6 mm,5μm）,以2%醋酸铵-甲醇（40∶60）为流动相,检测波长为225 nm,外标法计算含量。结果：丙谷胺在2.60-208.10μg与峰面积有良好的线性关系,r=0.999 9,平均加样回收率为99.8%,RSD为0.5%（n=6）。结论：HPLC法测定复方丙谷胺片中丙谷胺含量准确度高,操作简单,重复性好。     

高效液相色谱法测定百安洗液中盐酸小檗碱含量

目的建立百安洗液中盐酸小檗碱含量高效液相测定方法。方法色谱柱为Agilent Eclipse XDB-C18(5μm,4.6×150mm),流动相为乙腈-水-磷酸二氢钾-十二烷基磺酸钠(50∶50∶0.34∶0.17),流速1.0mL/min,测定波长为346nm。结果线性范围为0.0584~0.3504μg(r=0.9999),平均回收率为98.10%,RSD=1.66%(n=6),精密度RSD=1.23%(n=6),重复性RSD=1.82%(n=6)。结论方法简便、稳定、可靠,可用于百安洗液中盐酸小檗碱含量测定。     

高效液相色谱法测定龙连利胆合剂中2组分的含量

目的:建立以高效液相色谱法测定龙连利胆合剂中大黄素、龙胆苦苷含量的方法。方法:色谱柱为ShimpackC18(150mm×6mm,5μm)。测定大黄素的流动相为甲醇-水-磷酸(850∶150∶0.3),检测波长为287nm;测定龙胆苦苷的流动相为甲醇-水(3∶7),检测波长为258nm。流速均为1.0mL.min-1。结果:大黄素的平均回收率为102.8%(RSD=1.7%,n=9),线性范围为0.05~0.25μg;龙胆苦苷的平均回收率为96.4%(RSD=1.7%,n=9),线性范围为0.125~1.0μg。结论:本方法准确、重现性好,可用于龙连利胆合剂的质量控制。     

HPLC法测定复方降压胶囊中氢氯噻嗪、地巴唑、氯氮(艹卓)和盐酸异丙嗪的含量

目的:建立离子对高效液相色谱法同时测定复方降压胶囊中氢氯噻嗪、地巴唑、氯氮(艹卓)和盐酸异丙嗪含量。方法:分析柱为 Hypersil C_(18)(4.6mm×250mm,5μm),流动相为乙腈-甲醇-7.2mmol·L~(-1)己烷磺酸钠溶液-冰醋酸-三乙胺(28∶28∶43∶1∶0.01),检测波长为258nm。结果:氢氯噻嗪、地巴唑、氯氮(艹卓)和盐酸异丙嗪的线性范围分别为12.24-122.4μg·mL~(-1)(r=0.9997),40.92-409.2μg·mL~(-1)(r=0.9998),8.12-81.2μg·mL~(-1)(r=0.9999),11.52-115.2μg·mL~(-1)(r=0.9999);平均回收率分别为100.3%(RSD<1.4%),99.0%(RSD<1.3%),98.8%(RSD<1.7%),99.4%(RSD<2.3%)。结论:4种组分分离效果好,其他组分和辅料无干扰,本法简便快速,准确可靠,适于该复方制剂中4种组分的同时测定。     

HPLC法测定金蒲胶囊中苦参碱的含量

目的:建立高效液相色谱法测定金蒲胶囊中苦参碱的含量。方法:采用ZorbaxC18色谱柱(4.6mm×250mm,5μm),流动相为甲醇-乙腈-磷酸盐缓冲液(PH6.8)-三乙胺(18∶18∶70∶0.1),流速1.0mL·min-1,检测波长220nm。结果:进样量在0.2116μg～1.2696μg范围内呈良好线性关系,其回归方程为Y=1105738.7X-4017.1(r=0.9999)。平均回收率98.6%(n=6),RSD=2.4%。结论:该法简便、灵敏、准确,重现性好,可用作含量测定。     

HPLC法测定卡培他滨的含量及有关物质

目的建立高效液相色谱法测定卡培他滨含量及有关物质的方法。方法采用C18柱,以B(甲醇∶乙腈∶0.1%醋酸=7∶0.2∶12.8)-C(甲醇∶乙腈∶0.1%醋酸=16∶1∶3)为流动相,梯度洗脱,流速为1.0mL.min-1,进样量为10μL,检测波长为250nm,柱温为40℃,自动进样室为5℃。结果在浓度为0.0997~0.997mg.mL-1范围内线性关系良好(r=0.9999,n=6),检测限为0.020μg.mL-1。该方法能够分离卡培他滨及其有关物质。结论本方法灵敏、准确、专属性及重复性好,可用于卡培他滨的含量测定及有关物质限量检查。     

HPLC-ELSD测定肠外营养用海豹油脂肪乳中溶血磷脂酰胆碱的含量

目的建立HPLC-ELSD测定肠外营养用海豹油脂肪乳中溶血磷脂酰胆碱的含量。方法采用硅胶色谱柱(MZ-ANALYTICAL Spherisorb,250 mm×4.6 mm,5μm),流动相A为甲醇-水-冰醋酸-三乙胺(850∶1 50∶4.5∶0.5),流动相B为甲醇-水-冰醋酸-三乙胺-正己烷-异丙醇(385∶68∶2∶0.23∶1 60∶3 84),等度洗脱,A∶B=30∶70,流速为1.0mL.min1;进样体积为20μL,柱温为40℃;蒸发光散射检测器,漂移管温度为70℃,雾化气为氮气,气体流量为2 L.min1。结果线性范围为0.02~0.4 mg.mL1(r=0.999 4),检测限为0.12μg(S/N=3),定量限为0.40μg(S/N=10,n=3),平均回收率为100.3%,RSD为0.54%(n=9)。结论该方法灵敏、快速、准确、重复性好、专属性强,可用于本制剂的质量控制。     

高效液相色谱法测定人血浆中阿莫地喹的浓度(英文)

目的:建立高效液相色谱法测定人血浆中阿莫地喹的浓度。方法:分析柱采用KromasilC18(150mm×4.6mm,5μm),流动相为甲醇∶水∶三乙胺∶磷酸∶(21∶77.5∶1∶0.5),流速为1.0mL·min-1,检测波长为294nm,内标为羟氯喹。结果:阿莫地喹和羟氯喹的保留时间分别为5.82min,8.56min。该法在10～1000μg·L-1浓度范围内有良好的线性关系(r=0.9998,n=9),最低检测限为5μg·L-1,提取回收率为75.5%～82.7%,方法回收率为97.0%～104.8%。日内精密度的RSD<6.0%,日间精密度的RSD<7.5%。结论:该法简单,灵敏适合于阿莫地喹的药动学研究。     

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.     

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.     

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.