紫外分光光度法测定双氯芬酸钠滴眼液的含量

<正> 双氯芬酸钠为目前国内外广泛使用的非甾体抗炎药。其片剂和注射液的含量测定,广东省药品标准已有收载,本文介绍用紫外分光光度法测定双氯芬酸钠的含量,操作简便、快速,重现性好,结果满意。 一、仪器与药品 紫外分光光度计(日本岛津uv—3000) 乙醇(分析纯) 双氯芬酸钠对照品购自上海第十五制药厂 双氯芬酸钠滴眼液为自制 二、实验条件 1.双氯芬酸钠的紫外吸收光谱取双氯芬酸钠对照品适量,用乙醇制成每ml含10μg     

反相HPLC同时测定复方诺氟沙星滴眼液中诺氟沙星和地塞米松磷酸钠的含量及有关物质

目的 建立反相高效液相色谱法测定复方诺氟沙星滴眼液中诺氟沙星和地塞米松磷酸钠的含量及有关物质.方法 使用反相高效液相色谱法.用资生堂SHISEIDO C18(UG120,4.6mm×250mm,50m)色谱柱;以醋酸铵高氯酸钠溶液(取醋酸铵2.4g和高氯酸钠4.2g,用水900mL使溶解,用磷酸调pH值至2.5,再加水稀释至1000mL).乙腈-甲醇(68:22:10)为流动相;检测波长有关物质为278nm,地塞米松磷酸钠含量测定为242nm,诺氟沙星含量测定为278nm.结果 诺氟沙星的最低检测限为0.5ng;诺氟沙星在12.1～120.8μg/mL、地塞米松磷酸钠在2.1-21.2μg/mL的范围内浓度与峰面积呈良好的线性关系,线性回归方程分别为A=69068C-1619(r=1.000)和A=25580C+382(r=1.000);两组分的回收率分别为100.01%和99.87%,相对标准偏差(RSD)为0.4%和0.4%.结论 本方法灵敏、准确、专属性强可用于测定复方诺氟沙星滴眼液中两组分的含量和有关物质.     

RP-HPLC法测定双氯芬酸钠注射液的含量和有关物质

目的:建立同时测定双氯芬酸钠注射液含量及其有关物质的HPLC方法.方法:采用Phenomenex Luna C8色谱柱(4.6mm× 250 mm,5μm),流动相为磷酸盐缓冲液(0.01 mol·L-1磷酸溶液和0.01 mol·L-1磷酸二氢钠溶液等体积混合,必要时以其中一种溶液调节pH值至2.5)-甲醇(34∶66),流速1.0 mL·min-1,检测波长246 nm,柱温30℃,进样量10μL.结果:双氯芬酸钠的进样量在761.8 ～7 618 ng范围内,与峰面积呈良好的线性关系(r=1.000 0),平均回收率(n=9)为100.1％,RSD为0.5％;双氯芬酸钠杂质A的进样量在10.82～108.24 ng范围内,与峰面积呈良好的线性关系(r=0.999 9),双氯芬酸钠和双氯芬酸钠杂质A的最小检出量分别为3.0ng,1.4ng.结论:本方法简便、准确、灵敏、重现性好,专属性强,可用于双氯芬酸钠注射液的质量控制.     

HPLC法测定复方双氯芬酸钠注射液中双氯芬酸钠和对乙酰氨基酚的含量

目的建立复方双氯芬酸钠注射液中双氯芬酸钠和对乙酰氨基酚的含量测定方法。方法采用反相高效液相色谱法,以十八烷基硅烷键合硅胶为填充剂(250mm×4.6mm,5μm),以甲醇-水(68∶32)为流动相(以冰醋酸调pH值至4.0);检测波长为275nm。结果双氯芬酸钠线性范围为0.05~0.5g·L-1,回收率为99.5%,RSD为0.8%(n=9);对乙酰氨基酚线性范围3.0~30g·L-1,回收率99.9%,RSD为0.5%(n=9)。结论该测定方法可为复方双氯芬酸钠注射液的质量控制提供依据。     

双氯芬酸钠滴眼液中苯扎氯铵的测定

目的采用HPLC双氯芬酸钠滴眼液中苯扎氯铵的含量。方法乙腈-5 mmol.L-1醋酸铵溶液（含1%三乙胺,用冰醋酸调节pH值至5.0±0.5）（65∶35）为流动相,CNW色谱柱（150 mm×4.6 mm,5μm）,检测波长为214 nm。结果苯扎氯铵的测定在12.50～125.00μg.mL-1与峰面积线性关系良好,苯扎氯铵的平均回收率为99.0%,RSD为1.3%。结论方法简单、灵敏度高,可用于双氯芬酸钠滴眼液中苯扎氯铵的测定。     

HPLC法测定双氯芬酸钠凝胶中双氯芬酸钠的含量

目的采用HPLC法测定双氯芬酸钠凝胶中双氯芬酸钠的含量。方法以十八烷基键合硅胶为填充剂;用甲醇-0.005 mol/L磷酸二氢钾溶液(p H=3.8)(70∶30)为流动相;检测波长:280 nm;流速:1.0 m L/min;外标法测峰面积定量。结果双氯芬酸钠在15.90~55.41μg/m L(r=0.999 0)范围内线性关系良好,平均回收率为100.48%,RSD为1.28%。结论本方法简便、快速、准确,可用于双氯芬酸钠凝胶中双氯芬酸钠的含量测定。     

双氯芬酸胆碱滴眼液的制备和含量测定

目的 :制备双氯芬酸胆碱滴眼液并测定其含量。方法 :利用双氯芬酸胆碱水溶液在 2 76nm波长处有最大吸收 ,用紫外分光光度法测定其含量。观察了该滴眼液的稳定性和刺激性。结果 :双氯芬酸胆碱在 5 .0× 10 -6 ～3 .5× 10 5mol·L-1浓度范围内呈良好的线性关系 ,平均回收率为 99.8% ,RSD =1.3 7% (n =5 ) ;且稳定性良好。结论 :该滴眼液疗效明显 ,无刺激性 ,测定方法简便、快速、准确     

HPLC法测定双氯芬酸钠凝胶的含量及有关物质

目的建立高效液相色谱法测定双氯芬酸钠凝胶的含量及有关物质。方法采用C18色谱柱(4.6 mm×250mm,5μm),以甲醇-水-冰醋酸(80∶20∶0.8)为流动相;检测波长为276nm,流速1.0mL.min-1。结果双氯芬酸钠在30~70μg.mL-1范围内吸收度与浓度的线性关系良好,r=0.9997;平均回收率为99.88%,RSD:0.24%,3批样品的含量分别为:99.64%,99.94%,99.97%,检测限为5ng.mL-1(S/N≈3)。有关物质为:0.087%,0.097%,0.099%。结论该法快速,简便,结果准确,适用于该制剂的质量控制。     

高效液相色谱法测定复方地塞米松滴眼液中地塞米松的含量

目的测定复方地塞米松滴眼液中有效成分地塞米松磷酸钠的含量.方法采用反相高效液相色谱(RP-HPLC)法,固定相为Nova-pak C18反相柱(4μm,3.9mm×250mm,大连依利特科技有限公司),流动相为甲醇-0.34%磷酸二氢钾溶液(6040);检测波长240nm;柱温30℃.结果线性范围为40.09～501.10μg(r=0.9999),平均回收率为98.97%,RSD=1.38%(n=6).结论RP-HPLC法可用于复方地塞米松滴眼液的质量控制.     

HPLC法测定氯双滴眼液中氯霉素和双氯芬酸钠含量

氯双滴眼液为新型广谱抗菌消炎滴眼液,用消炎镇痛药物双氯芬酸钠替代原氯地滴眼液中的地塞米松磷酸钠,没有激素类药物不良反应,副作用大大减轻,可长期用于治疗沙眼、急慢性结膜炎、麦粒肿等.主要成分为氯霉素、双氯芬酸钠,含有硼酸、硼砂缓冲溶液.因氯霉素和双氯芬酸钠在UV区光谱曲线重叠,不能用紫外法同时测定,而用HPLC法可同时测定此两种成分的含量,结果可靠,方法简便,可用于该制剂的质量控制.     

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.