阿莫西林颗粒中有关物质高效液相色谱分析方法的建立

目的 建立高效液相色谱法测定阿莫西林颗粒中的有关物质。方法 2021年6月至2022年2月,采用高效液相色谱法,色谱柱为Agilent Zorbax SB-C8(4.6 mm×250 mm,5μm);流动相A为0.05 mol/L磷酸缓冲液（取0.05 mol/L磷酸二氢钾溶液,用20%氢氧化钠溶液调节pH至5.5）,流动相B为0.05 mol/L磷酸缓冲液（取0.05 mol/L磷酸二氢钾溶液,用20%氢氧化钠溶液调节pH至4.5）-乙腈（84∶16）;进行梯度洗脱;检测波长为230 nm;流速为2.0 mL/min。结果 建立了用于分析阿莫西林颗粒中有关物质的高效液相色谱方法,该方法下主峰与各杂质峰间分离良好,各杂质成分在各自线性范围内与峰面积线性关系良好（r≥0.999）,专属性、重复性、精密度、稳定性、耐用性均符合要求。结论 该法专属性强、准确度和重复性好,可作为检测阿莫西林颗粒中有关物质的有效方法。     

高效液相色谱法测定阿莫西林/氟氯西林钠胶囊溶出度

目的:建立阿莫西林/氟氯西林钠胶囊溶出度测定方法.方法:采用转篮法,以水为溶剂,转速为100r/min.高效液相色谱法,以C1s柱为色谱柱,以用磷酸调pH值至2.6的0.1 mol/L磷酸二氢钾-0.018 mol/L十二烷基硫酸钠-甲醇-乙腈(275:275:200:250)溶液为流动相,检测波长为225 nm.结果:阿莫西林与氟氯西林的线性范围均为0.03～0.60 mg/mL, r=0.999 9;平均加样回收率阿莫西林为99.8%,RSD=0.8%(n=9),氟氯西林为99.9%,RSD为1.3%(n=9).结论:高效液相色谱法简便、准确、灵敏度高.     

国产注射用阿莫西林钠中主要杂质分析

目的:对国产注射用阿莫西林钠中的主要杂质进行分析。方法:采用高效液相色谱法,以Waters Nova-pak C18(250 mm×4.6 mm,5μm)为色谱柱,检测波长为254 nm,梯度洗脱检查105批样品的有关物质。结果:在国产注射用阿莫西林钠中共检出19个杂质,其中主要杂质为阿莫西林青霉氧酸、二酮哌嗪阿莫西林、阿莫西林二聚体和阿莫西林三聚体,单个杂质含量均小于3%,总杂质含量均小于6%。结论:本研究结果对进一步指导该品种生产有重大意义。     

高效液相色谱法测量药物中阿莫西林含量的分析

目的:关于高效液相色谱法测量药物中阿莫西林含量的分析.方法:通过高效液相色谱法测量系统,对其参数测量以及检验,并观察以及分析检验结果,并对高效液相色谱法测量阿莫西林含量中的可行性实施有效验证.结果:在0.48mg/mL～44mg/mL范围内,阿莫西林浓度、峰面积两者有一定相关性.检验结果还可看出,本研究药物以及阿莫西林身的回收率各为在87.2％与98.1％之间、100.24％.结论:高效液相色谱法测量各项药物中阿莫西林含量,可使得阿莫西林回收率达到100.24％,值得推荐.     

阿莫西林胶囊热降解聚合物杂质的2D-HPLC分析及质谱裂解机理探讨

目的:建立阿莫西林胶囊中热降解聚合物杂质的分析方法.方法:采用高效凝胶排阻色谱法(HPSEC法),使用 Shimpack Bio Diol-60(4.6 mm×300 mm,3 μm)二醇基高纯硅胶色谱柱,进样量为20 μL并以254 nm为检测波长,进行阿莫西林和聚合物杂质的分离.通过优化HPSEC中流动相pH、缓冲...     

薄层色谱法检查磷酸伯氨喹的有关物质及对映异构体的研究

目的:建立磷酸伯氨喹的有关物质检查法及鉴定其对映异构体.方法:采用薄层色谱法常用的硅胶GF254薄层板,以醋酸乙酯-异丙醇-浓氨溶液(43:35:5)为展开剂,以自身对照法检查磷酸伯氨喹原料的有关物质.采用正相高效液相色谱法,以Waters 5 μm硅胶柱为色谱柱,检测波长为261 nm,流动相为氯仿-正己烷-甲醇-浓氨溶液(45:45:10:0.1),流速为2 mL/min,确认其对映异构体.结果:有关物质均能达到较好分离,最低检出限可达0.3μg.薄层色谱中主斑点上方杂质斑点经鉴定为其对映异构体.结论:薄层色谱法较<英国药典>的高效液相色谱法更简便、快速,灵敏度较高,适用于磷酸伯氨喹的有关物质检查.     

HPLC法同时测定琥珀酸曲格列汀中9个杂质的含量

目的:建立高效液相色谱法同时测定琥珀酸曲格列汀中9个杂质的含量.方法:采用Welch Utimate AQ C18(4.6 mm×250 mm,5μm)色谱柱,以0.1％磷酸溶液-乙腈为流动相,梯度洗脱,流速1.0 mL·min-1,柱温35℃,检测波长230 nm.结果:该药与已知杂质Ⅰ～Ⅸ色谱峰之间的分离度良好;该...     

高效液相色谱法测定克林霉素磷酸酯片的溶出度

目的:用高效液相色谱法测定克林霉素磷酸酯片的溶出度.方法:采用转篮法测定克林霉素磷酸酯片的溶出度,以高效液相色谱法测定其浓度.色谱柱为RP-C18柱(5μm,200 mm×4.6 mm),流动相为0.1 mol/L磷酸二氢钾溶液-乙腈(775:225),流速为1.0 mL/min,检测波长为210 nm,室温下测定.结果:在0.04～1.00 mg/mL的浓度范围内,线性关系良好(r=0.999 2),平均回收率为100.0%,RSD为0.88%.结论:高效液相色谱法分析速度快,结果准确,适用于克林霉素磷酸酯片溶出度的测定.     

清热解郁颗粒的质量控制方法研究

目的建立清热解郁颗粒的质量控制方法.方法采用薄层色谱法对清热解郁颗粒中的赤芍、大黄进行定性鉴别;并采用高效液相色谱法对制剂中的葛根素进行含量测定.液相色谱条件ZOBAX SB-C18(4.6 mm×250 mm,5 μm)色谱柱,以甲醇-0.1%磷酸水溶液(23∶77)作为流动相,流速为1.0 mL·min-1,柱温30℃,检测波长为250 nm.结果薄层色谱图斑点清晰,阴性对照无干扰;高效液相色谱法精密度高、重复性良好,平均加样回收率为95.89%,RSD为0.61%.结论本方法快速简便,结果准确,可用于控制清热解郁颗粒的质量.     

金桑颗粒的质量标准研究

目的 建立金桑颗粒的质量标准.方法 2016年1—5月,采用薄层色谱法(TLC)对金桑颗粒处方中连翘及黄芩进行定性鉴别研究;高效液相色谱法(HPLC)对金桑颗粒中黄芩苷进行含量测定研究,以依利特Hypersil ODS2(4.6 mm×250 mm,5μm)为色谱柱;以甲醇-0.1％磷酸(47:53)为流动相;检测波长...     

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.     

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.     

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.