高效液相色谱法测定复方氨基酸(15)双肽(2)注射液中2种杂质的含量测定

目的:建立同时测定复方氨基酸(15)双肽(2)注射液中焦谷氨酸和环(甘氨酰-谷氨酰胺)含量的HPLC方法。方法:使用Aglient ZORBAX SB-C18色谱柱(250 mm×4.6 mm,5μm),流动相为0.01 mol.L-1磷酸氢二铵溶液(用磷酸调节pH至1.6),流速为1.0 mL.min-1;紫外检测波长为205 nm;柱温为15℃;进样量为50μL。结果:焦谷氨酸和环(甘氨酰-谷氨酰胺)浓度分别在25.15~503.0 mg.L-1和40.1~802.0 mg.L-1范围内线性关系良好,最低检测限(S/N=3)分别为75.45 ng和40.1 ng,平均回收率分别为100.9%和100.8%。结论:本方法用于复方氨基酸注射液中焦谷氨酸和环(甘氨酰-谷氨酰胺)含量的快速分析,方法简便、准确。     

HPLC法测定安神补脑液中防腐剂的含量

目的:建立测定安神补脑液中防腐剂含量的方法。方法:采用高效液相色谱法。色谱柱为Agilent Zorbax SB-C_(18),流动相为乙腈-0.05%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为236 nm,柱温为30℃,进样量为10μL。结果:苯甲酸和羟苯乙酯检测质量浓度线性范围分别为12.85～128.54μg/mL(r=0.999 9)、4.05～40.48μg/mL(r=0.999 8);定量限分别为0.514、1.012μg/mL,检测限分别为0.171、0.353μg/mL;精密度、稳定性、重复性试验的RSD<1.0%;加样回收率分别为99.38%～100.21%(RSD=0.31%,n=6)、97.96%～100.72%(RSD=0.91%,n=6)。结论:该方法操作简单、结果准确,可用于安神补脑液中防腐剂的含量测定。     

酢浆草的HPLC指纹图谱建立及2种有效成分的含量测定

目的:建立酢浆草的高效液相(HPLC)指纹图谱,并同时测定其中异牡荆素、当药黄素的含量。方法:采用HPLC法。色谱柱为ACE Excel-5-C₁₈,流动相为甲醇-0.1%磷酸水溶液(梯度洗脱),流速为1 mL/min,柱温为35℃,检测波长为280 nm,进样量为10μL。以异牡荆素峰为参照,绘制12批酢浆草药材样品的HPLC指纹图谱,采用《中药色谱指纹图谱相似度评价系统(2012版)》进行相似度评价,确定共有峰。按上述色谱条件同法测定异牡荆素、当药黄素的含量。结果:12批酢浆草药材样品共有19个共有峰,相似度均大于0.89,同时指认异牡荆素、当药黄素2个共有峰。异牡荆素、当药黄素检测质量浓度的线性范围分别为3.91～117.36μg/mL(r=0.999 4)、9.88～118.56μg/mL(r=0.999 2);定量限分别为0.675、3.587μg/mL;检测限分别为0.205、1.087μg/mL;精密度、重复性、稳定性试验的RSD均小于2%;加样回收率分别为95.46%～99.10%(RSD=1.23%,n=6)、95.34%～101.23%(RSD...     

高效液相色谱法同时测定骨松宝丸中5种成分含量

目的 建立同时测定骨松宝丸中5种成分含量的高效液相色谱(HPLC)法。方法 色谱柱为Diamonsil C₁₈柱(150 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为210 nm(淫羊藿苷、川续断皂苷Ⅵ、吉马酮)、233 nm(芍药苷、阿魏酸),柱温为30℃,进样量为10μL。结果 淫羊藿苷、川续断皂苷Ⅵ、芍药苷、阿魏酸和吉马酮质量浓度分别在10.180～203.60μg/mL(r=1.000 0),0.522～10.44μg/mL(r=0.999 9),1.274～25.47μg/mL(r=0.999 6),1.260～25.20μg/mL(r=0.999 6),0.517～10.34μg/mL(r=0.999 8)范围内与峰面积线性关系良好;定量限分别为0.33,0.44,0.09,0.11,0.39μg/mL;精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率分别为98.69%,95.88%,98.09%,97.68%,96.97%,RSD分别为1.66%,3.89%,2....     

离子色谱直接提取法测定天花粉中二氧化硫的含量

目的：建立离子色谱直接提取法测定天花粉中二氧化硫（SO2）含量的实验方法。方法采用氢氧化钾溶液（25 mmol/L）直接提取,色谱柱为AS11-HC色谱柱（4 mm×250 mm,9.0μm）;柱温20℃;淋洗液：氢氧化钾溶液（20 mmol/L）;淋洗液流速1.00 mL/min;电导检测法,电导池温度20℃通过分离度实验、精密度实验、重复性实验检测并计算分离度、亚硫酸根峰面积和天花粉中SO2含量及亚硫酸根峰面积与进样量的关系。结果亚硫酸根色谱峰与其他相邻色谱峰间有较好的分离度,峰面积变化不大,亚硫酸根平均含量为每克天花粉含SO20.1977 mg、RSD为0.6%。亚硫酸根标准溶液进样量在1.16～29.1μg（即当进样体积为100μL时,被测定溶液浓度为11.6～291.2μg/mL）与亚硫酸根色谱峰的峰面积有良好的线性关系,平均回收率为99.2%,最低定量限以被测定溶液计算为0.00138μg/mL。结论离子色谱法操作简便、准确、快速,适用于天花粉中SO2的定量检测。     

HPLC法同时测定复方利血平片中苯磺酸氨氯地平和缬沙坦含量

目的:建立复方利血平片中苯磺酸氨氯地平和缬沙坦含量的测定方法。方法:色谱柱:Agilent Eclipse Plus C18柱(5μm,4.6 mm×250 mm),进样量:20μL,柱温:室温;流动相:甲醇-0.2%磷酸(70∶30),流速:1.0 mL.min-1;检测波长:237 nm。结果:苯磺酸氨氯地平在0.017 34～0.173 4μg、缬沙坦在0.401 5～4.015μg范围内,对照品色谱峰面积与进样量呈良好的线性关系,相关系数r分别为0.999 94与0.999 99,平均回收率分别为99.2%(RSD=1.29%,n=6)与99.6%(RSD=0.71%,n=6)。结论:该法快速、简便、重现性好,可用于复方利血平片中苯磺酸氨氯地平和缬沙坦含量的测定。     

HPLC法测定委陵菜中黄酮类成分的含量

目的:建立HPLC法测定委陵菜中槲皮素、翻白叶苷A和芹菜素含量的方法.方法:色谱柱为ZORB-AXSB.C18色谱柱(4.6 mm×150 mm,5μm);流动相为甲醇-0.3%磷酸水溶液(51:49);检测波长为360 nm;流速为0.9 mL/min.结果:槲皮素、翻白叶苷A和芹菜素的进样量分别在0.72～10.08μg/mL、0.86～12.04μg/mL和0.54～7.56 μg/mL范围内与其峰面积呈良好的线性关系,线性系数均为0.999 9,平均回收率分别为95.37%、96.87%、97.66%,RqD分别为1.79%、1.63%、2.08%,药材中三中黄酮的含量分别为100.0μg/g、323.0μg/g和55.0μg/g;结论:该方法快速、简便、可靠,适用于委陵莱中黄酮类成分的含量测定.     

离子色谱法测定复方氨基酸注射液(20AA)中醋酸根

目的建立以氢氧根作为淋洗液的离子色谱法测定复方氨基酸注射液(20AA)中醋酸根的方法。方法使用Dionex ICS 3000离子谱仪,Dionex As19-Ag19阴离子交换色谱柱(250 mm×4 mm),水–30 mmol/L氢氧化钠溶液为淋洗液,梯度洗脱,体积流量1.0 mL/min,柱温30℃,进样量20μL,抑制型电导检测器,检测池温度35℃。结果醋酸根与相邻杂质的分离度为1.8,最低检出浓度0.75μmol/L,线性范围0.75~2.24 mmol/L(r=0.999 5),平均回收率为100.7%,RSD值为1.7%。结论该方法操作简单,分离度好,背景低,是控制复方氨基酸注射液(20AA)中醋酸根的可靠方法。     

高效液相色谱法测定复方甘草酸单铵系列注射剂中乙二胺四乙酸二钠含量

目的 建立快速测定复方甘草酸单铵系列注射剂中乙二胺四乙酸二钠(EDTA-2Na)含量的高效液相色谱(HPLC)法。方法 色谱柱为Hypersil GOLD C₁₈柱(250 mm×4.6 mm,5μm),流动相为50 mmol/L磷酸二氢钠溶液(含5 mmol/L四丁基溴化铵,用磷酸溶液调pH至4.5)-乙腈(90∶10,V/V),流速为1.0 mL/min,检测波长为257 nm,柱温为40℃,进样量为10μL。结果 EDTA-2Na质量浓度在2～200μg/mL范围内与EDTA-Fe³⁺线性关系良好(R²=0.999 8,n=7);检测限为0.02μg/mL,定量限为0.06μg/mL;精密度、重复性、稳定性试验的RSD均小于2.0%;复方甘草酸铵注射液、复方甘草酸单铵注射液、复方甘草酸单铵S氯化钠注射液、甘草酸单铵半胱氨酸氯化钠注射液、注射用复方甘草酸单铵S的平均回收率分别为100.57%,100.90%,100.86%,100.95%,101.03%,RSD分别为0.21%,0.82%,0.60%,0.64%,0...     

HPLC法测定复方氨基酸（15）双肽（2） 注射液中有关物质的含量

目的：建立测定复方氨基酸（15）双肽（2）注射液中有关物质含量的高效液相色谱法。方法：采用Ultimate AQ-C18（250mm *4.6mm,5µm）色谱柱,以0.01mol?L-1磷酸氢二铵溶液（pH2.0）-甲醇（98：2）为流动相,流速为0.7mL?min-1,检测波长为205nm,进样量为50µL。结果：在选定的色谱条件下,环-（甘氨酰谷氨酰胺）峰、焦谷氨酸峰和环-（甘氨酰酪氨酸）峰与各自相邻色谱峰可以有效分离;环-（甘氨酰谷氨酰胺）、焦谷氨酸、环-（甘氨酰酪氨酸）分别在7.863～52.42µg?mL-1、5.256～35.04µg?mL-1、0.9393～6.262µg?mL-1的范围内线性关系良好（r=0.9999）;精密度试验的RSD值均小于0.2%;重复性试验的RSD值均小于2.0%;环-（甘氨酰谷氨酰胺）、焦谷氨酸和环-（甘氨酰酪氨酸）定量限分别为3.15、14.0和7.5ng,检测限分别为0.95、7.0和2.5ng;加样回收率分别为103.0、101.5和103.3%（n=9）,RSD值分别为1.0%、0.9%和0.9%。结论：该方法专属性强,结果准确,可用于复方氨基酸（15）双肽（2）注射液中有关物质的测定,能有效的反应药品质量。     

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.     

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.     

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.