高效液相色谱法测定阿奇霉素葡萄糖注射液含量

目的建立高效液相色谱法测定阿奇霉素葡萄糖注射液的含量.方法以CN-3柱为分析柱,以0.045 mol·L-1磷酸二氢铵-乙腈(6040,v/v)为流动相,0.2%的三乙铵调节pH约为7.0;柱温40℃;检测波长210nm.峰面积外标法定量.结果0.4～4 g·L-1浓度范围内呈现良好线性关系,r=0.999 9,平均回收率为99.4%,RSD为0.15%(n=3).结论本方法操作简便、快速,结果准确可靠,重现性好,可用于测定阿奇霉素葡萄糖注射液的含量.     

高效液相色谱法测定阿奇霉素干混悬剂中阿奇霉素的含量

目的:建立高效液相色谱法测定阿奇霉素干混悬剂含量的方法。方法:Venusil XBP-C18(L)(150mm×4.6mm,5μm)柱为固定相,0.05mol·L-1磷酸氢二钾(20%的磷酸溶液调节pH值至8.2)-乙腈(45∶55)为流动相,进样量为20μL,流速为1.2mL·min-1,紫外检测波长为210nm。结果:阿奇霉素主成分峰与相邻杂质峰分离度>1.5。阿奇霉素检测浓度在10～5000μg·mL-1内与峰面积积分值呈良好线性关系(r=0.9999);平均回收率为98.83%,RSD=0.54%(n=6),日内、日间与中间精密度均<2.5%。结论:本法专属性强、准确,可用于测定阿奇霉素干混悬剂的含量。     

高效液相色谱法测定阿奇霉素葡萄糖注射液的含量

目的 采用高效液相色谱法（HPLC法）测定阿奇霉素葡萄糖注射液的含量。方法 以phenomenex C18柱为分析柱，流动相为乙腈-水（80：20），流速为1．0mL／min，检测波长为205nm，柱温为40℃；以峰面积外标法计算含量。结果 阿奇霉素葡萄糖注射液浓度在0.5～5g／L浓度范围内与峰面积线性关系良好，r=0．9972，平均回收率为99.8％，RSD=0．9％（n=6）。结论 HPLC法操作简便、快速，结果准确可靠，重现性好，可用于测定阿奇霉素葡萄糖注射液的含量。     

HPLC法测定克林霉素磷酸酯注射液中抑菌剂苯甲醇的含量

目的:建立高效液相色谱法测定克林霉素磷酸酯注射液中抑菌剂苯甲醇含量的方法。方法:采用色谱柱为CAPCELL PAKC8,流动相为磷酸二氢钾溶液-乙腈(775:225),流速为1.0mL·min~(-1),检测波长为210nm。结果:苯甲醇检测浓度线性范围为4.175～41.75μg·mL~(-1)(r=0.9999),平均加样回收率为100.5%(n=9),RSD=0.09%。结论:本方法准确、重复性好,可用于克林霉素磷酸酯注射液中苯甲醇含量的测定。     

UPLC-MS法测定人血浆中阿奇霉素的浓度

目的:建立测定人血浆中阿奇霉素浓度的方法。方法:采用直接沉淀法处理血浆后以超高效液相色谱-串联质谱(UPLC-MS)法进样测定。色谱柱为Waters Acquity UPLC BEH C18流动相为乙腈-10 mmo·lmL-1甲酸铵水溶液(66∶34),流速为0.2 mL·min-1;正离子多离子反应监测(MRM)扫描分析,离子通道分别为m/z 748.36→591.10(阿奇霉素)、m/z 837.34→158.06(罗红霉素)。结果:阿奇霉素血药浓度在2～1 000 ng·mL-1范围内线性关系良好(r=0.999 5),定量下限为2 ng·mL-1平均方法回收率为102.6%～108.0%,平均提取回收率为93.2%～102.2%,日内、日间RSD均<8%。结论:本方法简便、快速、可靠、特异性强、灵敏度高,可用于阿奇霉素的药动学研究。     

高效液相色谱法测定阿奇霉素的含量

目的:用高效液相色谱法测定阿奇霉素的含量.方法:以日本岛津CLC-CN柱为固定相,0.1 mol·L-1磷酸二氢钠-甲醇-乙腈(85∶7∶8)为流动相,在pH 3.0～3.5,流速:1 mL·min-1,柱温:40 ℃,紫外检测波长210 nm,灵敏度为0.08 AUFS的条件下分离测定阿奇霉素,并对方法进行了认证.结果:阿奇霉素与其杂质能完全分离,在100～1 000 mg·L-1范围内,浓度与峰面积线性关系良好,r=0.999 6(n=3).阿奇霉素的平均回收率为100.3%(n=9),日内RSD在0.35%～3.90%之间(n=9),日间RSD在0.35%～4.40%(n=9),重复进样精度RSD%在2%以下(n=5).在pH 3～9之间的溶液中及3%双氧水中,阿奇霉素在12 h内含量基本保持不变.结论:本法简便、迅速、灵敏度高及重现性好,可用于测定阿奇霉素的含量.     

RP—HPLC法测定甲砜霉素及其胶囊剂的含量和有关物质

目的:采用反相高效液相色谱法测定甲砜霉素及其胶囊剂的含量及有关物质。方法:采用Merck C18色谱柱(250 mm×4.0 mm,5μm);以乙腈-水(1:4)为流动相;流速1.2 mL·min-1;检测波长:225 nm;柱温:30℃;进样量:10μL。结果:含量测定的线性范围为20.29—203.9 μg·mL～1,r=0.9999(n=7);有关物质测定的线性范围为2.072—20.72μg·mL-1;r=0.9998(n=7),甲砜霉素胶囊的加样回收率为101.3％,99.2％,98.9％;RSD依次为1.9％,0.4％,0.7％(n=3)。结论:本法简便快速、准确,专属性好。     

高效液相色谱-质谱联用法测定人体内血浆中的阿奇霉素

目的:建立一种简便、快速的高效液相色谱质谱联用法测定人体内血浆中的阿奇霉素浓度的方法。方法:采用HyPurityC18柱(2.1mm×150mm,5μm),柱温40°C,流动相为10mmol·L-1醋酸铵(pH5.2)∶乙腈∶甲醇(50∶40∶10),流速为0.2mL·min-1,质谱条件采用正离子检测的电喷雾接口(ESI),其喷雾电压4.5kV,选择性监测质荷比(M/Z)为375(阿奇霉素),749(克拉霉素)带正电荷的分子离子峰。结果:阿奇霉素最低定量限为3.91μg·L-1,线性范围3.91～1000μg·L-1(r=0.9993),日内和日间RSD均低于12%。结论:该方法灵敏度高、快速、简便、无杂质干扰,适合于阿奇霉素浓度检测以及生物等效性研究。     

RP—HPLC法测定香丹注射液中丹酚酸A的含量

目的:控制香丹注射液的质量。方法:建立高效液相色谱法测定香丹注射液中丹酚酸A的含量。色谱柱为Luna C_(18)(2)色谱柱(4.6mm×15cm,5μm),流动相为甲醇-水-甲酸(41:59:0.8),检测波长为285nm,流速为1.0mL·min~(-1),柱温25℃。结果:丹酚酸A进样量在0.24～5.6μg范围内线性良好,r=0.9997,理论板数5.5×10~3,方法平均回收率为101.3％。应用本法测定了5个厂家生产的香丹注射液,含量范围为0～1.148mg·mL~(-1)。结论:本法操作简单,结果可靠,可作为香丹注射液的常规检验方法。     

HPLC法电化学检测阿奇霉素片的有关物质

目的:建立以高效液相色谱法电化学检测阿奇霉素片中有关物质的方法。方法:色谱柱为Gamma ARP-1/P,流动相为0.014mol·L-1磷酸氢二钾/0.020mol·L-1氢氧化钠(用磷酸和氢氧化钠调pH至11)-乙腈(71∶29),流速为0.7mL·min-1,柱温为40℃,进样量为50μL,玻璃碳电极的检测电位为+900mV。结果:红霉素过氧化物、阿奇霉素脱氧化物、阿奇霉素杂质A和N脱甲基阿奇霉素进样量的线性范围分别为0.15~1.80(r=0.999)、0.09~1.08(r=0.999)、0.23~2.76(r=0.998)、0.30~3.60μg(r=0.998);平均回收率分别为98.9%(RSD=1.1%)、94.6%(RSD=5.4%)、103.4%(RSD=3.4%)、96.2%(RSD=4.3%),有关物质含量检测结果均<0.7%。结论:本方法重现性好、灵敏度高、结果稳定准确,可用于检测该制剂的有关物质。     

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.     

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.