HPLC梯度洗脱法测定对乙酰氨基酚异丙嗪注射液中的主药及对氨基酚

目的 采用HPLC法同时测定对乙酰氨基酚异丙嗪注射液中的对氨基酚、对乙酰氨基酚和盐酸异丙嗪.方法 采用Phenomenex C18柱(200 mm x4.6 mm、5μm),流动相为0.05 mol·L-1醋酸铵(A)-甲醇(B),梯度洗脱为0(85%A)→10 min(85%A) →11min(20%A)→30 min(20%A)→31min(85%A),二极管阵列检测,对氨基酚的测定波长为232nm、对乙酰氨基酚、盐酸异丙嗪的为253nm.结果 对氨基酚、对乙酰氨基酚和盐酸异丙嗪分离良好,三者的线性范围分别为5.2～104.6ng、0.23-4.67μg、0.26～5.10μg;r均为0.9999;平均回收率均为100.0%、100.4%、100.9%;RSD分别为1.3%、0.3%、0.8%(n=9).结论 所用方法结果准确,重复性良好,简便可行.     

多波长系数法测定散利痛片中3组分的含量

目的 建立简单快速测定散利痛片中对乙酰氨基酚、咖啡因、异丙安替比林含量的方法.方法 建立多波长系数法同时测定散利痛片中对乙酰氨基酚、咖啡因、异丙安替比林3组分的含量.结果 对乙酰氨基酚、咖啡因、异丙安替比林线性范围分别为4.00～14.0 μg·mL-1 (r=0.999 4),0.806～2.82 μg·mL-1(r=0.999 3),2.40～8.40 μg·mL-1 (r=0.999 2),平均回收率分别为100.1%,100.4%,101.1%,RSD分别为1.4%,1.6%,1.2%(n=9).结论 本法方便、快速、准确,适用于散利痛片生产过程中的快速质量控制.     

HPLC法测定小儿氨酚匹林咖啡因片中四种成分的含量

目的:建立HPLC法同时测定小儿氨酚匹林咖啡因片中对乙酰氨基酚、咖啡因、阿司匹林及水杨酸的含量.方法:采用岛津ODS-VP色谱柱(4.6 mm×150 mm,5μm);以甲醇-0.01mol·L-1磷酸溶液(30:70)(用三乙胺调节pH值至3.1)为流动相;检测波长为220nm;流速为1.0 mL·min-1.结果:在建立的色谱条件下,对乙酰氨基酚、咖啡因、阿司匹林、水杨酸的线性范围分别为12.6～126 nag·L-1(r=0.999 9);3.0～30.0 rag·L-1(r=1.000 0);23.0～230 mg·L-1(r=0.999 8);0.115～6.9 mg·L-1(r=1.000 0).对乙酰氨基酚、咖啡因、阿司匹林的平均回收率分别为99,1%(RSD=1.32%,n=9);100.0%(RSD=0.57%,m=9);99.0%(RSD=1.09%,n=9).结论:本法简便、快捷,准确度高,专属性强,重现性好,可用于小儿氨酚匹林咖啡因片中对乙酰氨基酚、咖啡因、阿司匹林的含量测定及水杨酸的限度控制.     

HPLC法同时测定小儿氨酚烷胺颗粒中3种成分的含量

目的建立同时测定小儿氨酚烷胺颗粒中对乙酰氨基酚、马来酸氯苯那敏、咖啡因的高效液相色谱含量测定方法。方法采用D iam onsil C18(4.6 mm×250 mm,5μm)色谱柱;甲醇-0.05 m ol/L磷酸二氢钾溶液(20∶80)(1%磷酸调pH3.0)为流动相;流速:1.0 m l/m in;检测波长:210 nm。结果对乙酰氨基酚的线性范围为0.490 2~29.412 0μg(r=1.000 0)、平均回收率(n=9)为100.3%,RSD为0.43%;马来酸氯苯那敏的线性范围为0.003 992~0.239 520μg(r=0.999 9),平均回收率(n=9)为100.5%,RSD为0.20%;咖啡因的线性范围为0.030 64~1.838 40μg(r=1.000 0),平均回收率(n=9)为100.5%,RSD为0.23%。结论本方法简便、结果准确,可用于制剂的含量测定和质量控制。     

HPLC法同时测定小儿氨酚烷胺颗粒中3种成分的含量

目的建立同时测定小儿氨酚烷胺颗粒中对乙酰氨基酚、马来酸氯苯那敏、咖啡因的高效液相色谱含量测定方法。方法采用D iam onsil C18(4.6 mm×250 mm,5μm)色谱柱;甲醇-0.05 m ol/L磷酸二氢钾溶液(20∶80)(1%磷酸调pH3.0)为流动相;流速:1.0 m l/m in;检测波长:210 nm。结果对乙酰氨基酚的线性范围为0.490 2~29.412 0μg(r=1.000 0)、平均回收率(n=9)为100.3%,RSD为0.43%;马来酸氯苯那敏的线性范围为0.003 992~0.239 520μg(r=0.999 9),平均回收率(n=9)为100.5%,RSD为0.20%;咖啡因的线性范围为0.030 64~1.838 40μg(r=1.000 0),平均回收率(n=9)为100.5%,RSD为0.23%。结论本方法简便、结果准确,可用于制剂的含量测定和质量控制。     

HPLC法同时测定感冒灵颗粒中对乙酰氨基酚、咖啡因和马来酸氯苯那敏的含量

目的建立HPLC法同时测定感冒灵颗粒中对乙酰氨基酚、咖啡因和马来酸氯苯那敏的含量。方法色谱柱为Welch Xtimate C18柱(5μm 4.6×250mm),以甲醇-1%醋酸(用二乙胺调节至pH 3.7)(38∶62)为流动相,流速为1.0mL·min-1,柱温为40℃,PDA检测器,波长260nm。结果对乙酰氨基酚、咖啡因、马来酸氯苯那敏的线性范围分别为49.90~499.0μg·mL-1(r=0.9997),1.028~10.28μg·mL-1(r=0.9999),1.087~10.87μg·mL-1(r=1.000),平均加样回收率(n=9)分别为98.71%(RSD 1.2%),99.17%(RSD1.4%),100.78%(RSD为1.6%)。结论本方法快速、简便、准确,重现性好,可作为控制感冒灵颗粒质量的方法。     

HPLC法同时测定复方氨酚烷胺片中对乙酰氨基酚和咖啡因的含量

目的建立复方氨酚烷胺片中对乙酰氨基酚和咖啡因的含量测定方法。方法用KromasilC18色谱柱(250×4.6mm,5μm),以0.1%醋酸溶液-甲醇(50:50)(用二乙胺调pH至3.7)为流动相,流速为1.0mL·min-1,检测波长为272nm。结果对乙酰氨基酚和无水咖啡因的线性范围分别为100.12～300.36μg·mL-1(r=0.9997)和5.51～16.54μg·mL-1(r=0.9999),平均回收率分别为99.3%,RSD=1.1%(n=5)和98.4%,RSD=0.5%(n=5)。结论本法适用于复方氨酚烷胺片中对乙酰氨基酚和咖啡因的含量测定。     

HPLC测定复方氨酚苯海拉明片中对乙酰氨基酚和咖啡因含量

目的建立高效液相色谱法测定复方氨酚苯海拉明片中对乙酰氨基酚和咖啡因的含量。方法采用KromasilC18色谱柱(4.5 mm×150 mm,5μm),流动相为甲醇-水(30∶70),流速为1.0 mL.min-1,检测波长为280 nm,柱温为室温,进样体积为20μL。结果对乙酰氨基酚和咖啡因的线性范围分别为80~320 mg.L-1(r=0.999 7,n=7)和10~30 mg.L-1(r=0.999 7,n=5);高中低3种浓度的平均回收率分别为100.7%(RSD=0.69%),101.3%(RSD=0.53%),n=9。结论本方法简便、准确、灵敏、回收率高。     

HPLC法同时测定氨麻苯美片中4种主要成分的含量

目的:建立同时测定氨麻苯美片中盐酸伪麻黄碱、对乙酰氨基酚、氢溴酸右美沙芬和盐酸苯海拉明等成分含量的HPLC方法。方法:色谱柱为Kromasil 60-5CN(25 mm×4.6 mm,5μm)柱;以乙腈-pH3.0的40 mmol.L-1三乙胺水溶液(20∶80)为流动相;检测波长为215 nm;流速为1.0 mL.min-1。结果:盐酸伪麻黄碱、对乙酰氨基酚、氢溴酸右美沙芬和盐酸苯海拉明的线性范围分别为6.036~150.9μg.mL-1(r=1.0000),65.42~1636μg.mL-1(r=0.9989),3.010~75.25μg.mL-1(r=1.0000),50.90~127.2μg.mL-1(r=1.0000);加样回收率(n=9)分别为98.5%,100.9%,99.1%和99.6%。结论:本法简单、快速、准确,可用于氨麻苯美片中4种主要成分的同时测定。     

HPLC法测定小儿咳喘灵颗粒中盐酸麻黄碱和盐酸伪麻黄碱含量

目的建立高效液相色谱法同时测定小儿咳喘灵颗粒中盐酸麻黄碱和盐酸伪麻黄碱含量的方法。方法采用反相高效液相色谱法,色谱柱为Agilent-ODS-3(5μm,4.6 mm×250 mm),以乙腈-0.1%磷酸溶液(5∶95)为流动相;检测波长为207 nm,流速为1.0 ml.min-1,柱温25℃。结果盐酸麻黄碱线性浓度范围在0.0306~0.306μg,r=0.999 9,平均回收率为99.52%,RSD=0.39%(n=9),盐酸伪麻黄碱线性浓度范围在0.0278~0.278μg,r=0.999 8,平均回收率为99.49%,RSD=0.52%(n=9)。结论本法简单准确,重复性好,可作为小儿咳喘灵颗粒的质量控制方法。     

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.     

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.