RP-HPLC法测定维生素B1,B2及B6片中含量

目的:建立一种反相高效液相色谱法测定,维生素B1、维生素B2、维生素B6的含量测定方法.方法:Hypersil, ODSC18柱(250mm×4.6mm,5μm),流动相:甲醇-50mmol·L-1磷酸二氢钾溶液(20:80),检测波长为266nm,流速1.0ml·min-1.结果:维生素B1、维生素B2、维生素B6;线性范围分别为:16.05～80.25μg·ml-1(r=0.9999)21.35～106.75μg·ml-1(r=0.9999)及14.15～70.75μg·ml-1(r=0.9999),平均回收率也分别为101.2%,98.7%及99.6%,RSD 1.9%,1.9%及1.0%.结论:该方法准确,灵敏度高,重现性好,可作为质量检验的定量方法.     

气相色谱法测定培美曲塞二钠中溶剂残留

建立气相色谱法分析培美曲塞二钠中溶剂残留。采用HP-1毛细管柱,以苯为内标进行定量。甲醇、二氯甲烷、乙醇、醋酸乙酯的线性范围分别为10.02~50.10μg.ml-1(r=0.9996),4.12~20.6μg.ml-1(r=0.9990),15.08~75.40μg.ml-1(r=0.9990),15.13~75.65μg.ml-1(r=0.9990),回收率分别为100.10%,100.25%,101.00%,100.93%,RSD分别为0.8%,1.3%,0.6%,0.9%。本方法简单、准确、灵敏度高、重现性好。     

HPLC测定香青兰药材中的黄酮类成分

目的 建立测定香青兰药材含量的方法.方法 采用HPLC测定.结果 所测香青兰药材中山奈素、洋芹素、异鼠李素,各成分的线性关系良好,其线性范围分别为6.06～60.60 μg·ml-1(r=0.9996)、3.04～30.40 μg·ml-1(r=0.9997)、2.64～26.40μg·ml-1(r=0.9996).其回收率分别为96.2%(RSD=1.1%)、96.9%(RSD=1.1%)、97.2%(RSD=1.2%)(n=3).结论 所建方法准确、简便,为科学地评价香青兰药材的质量提供了依据.     

大口径毛细管气相色谱法测定螺普利中5种残留的有机溶剂

目的 建立测定螺普利中5种有机溶剂残留量的方法.方法 采用大口径毛细管柱气相色谱法.结果 5种有机溶剂均可完全分离, 乙醇、乙醚、乙酸乙酯、苯、N,N-二甲基甲酰胺的线性范围分别为:1.84～3.68×103 μg · ml-1 (r=0.9993)、0.90～1.8×103 μg · ml-1 (r=0.9996)、1.56～3.12×103 μg · ml-1 (r=0.9998)、1.20～1.2×103 μg · ml-1 (r=0.9997)、3.81～3.81×103 μg · ml-1 (r=0.9995),平均回收率分别为99.2%、98.9%、99.5%、102.1%、101.3%,RSD分别为2.0%、1.9%、1.5%、2.5%、1.2%(n=5).结论 所建方法灵敏、准确,可用于螺普利中5种残留溶剂的同时测定.     

HPLC法测定复合维生素注射液(13种)中4种脂溶性维生素的含量

目的建立HPLC法同时测定复合维生素注射液(13种)中4种脂溶性维生素的方法.方法采用固相萃取法,分离4种脂溶性维生素,色谱柱Inetsil ODS2 C18柱(150 mm×4.6 mm,5μm),流动相乙腈-甲醇一二氯甲烷(801010),检测波长265 nm,流速1.0 ml·min-1,柱温30℃.结果维生素D3、维生素E、维生素K1及维生素A的线性范围分别为0.82～1.2μg·ml-1(0.999 6),1.65～2.48 mg·ml-1(0.999 8),240～360μg·ml-1(r=0.999 7)及O.16～0.24 mg·ml-1(r=0.999 5),平均回收率为100.7%(RSD1.2%),101.5%(RSD 1.9%),100.7%(RSD 1.1%)及99.3%(RSD0.9%)(n=9).结论方法简单、快速、重复性好,可用于该该剂的质量控制.     

高效液相色谱法测定脑塞通丸中人参皂苷Rg1、Re、Rb1的含量

目的建立脑塞通丸的含量测定方法.方法采用高效液相色谱法.色谱柱Agilent Technologies ZORBAX ExtendC18(250 mm×4.6 mm,5μm),流动相乙腈-0.05%磷酸溶液梯度洗脱,流速1.0 ml·min-1,检测波长203 nm,柱温35℃.结果人参皂苷Rg1在8.516～425.8μg·ml-1范围内线性关系良好(r=0.999 9),平均加样回收率为97.6%,RSD=1.7%(n=6);人参皂苷Re在20.06～1003μg·ml-1范围内线性关系良好(r=0.999 7),平均加样回收率为97.6%,RSD=2.0%(n=6);人参皂苷Rb1在19.456～972.8μg·ml-1范围内线性关系良好(r=0.999 7),平均加样回收率为96.8%,RSD=1.3%(n=6).结论该方法简便易行,结果准确可靠,可适用于脑塞通丸的质量控制.     

HPLC法同时测定宫炎平胶囊中没食子酸、槲皮素、山柰素的含量

目的:建立宫炎平胶囊中没食子酸、槲皮素和山奈素的含量测定方法。方法:应用高效液相色谱法测定,色谱柱为Agilent-SB C18(250 mm×4.6 mm,5μm),以甲醇和0.3%磷酸水溶液为流动相进行梯度洗脱,流速为1.0 ml·min-1,柱温30℃。结果:没食子酸、槲皮素和山奈素的线性范围分别为98.200~491.000μg·ml-1(r=0.999 9)、7.520~37.600μg·ml-1(r=0.999 9)、4.940~24.700μg·ml-1(r=0.999 9);平均加样回收率分别为96.74%(RSD=1.33%)、98.18%(RSD=1.70%)、97.04%(RSD=1.28%)结论:该方法简便易行、准确、重复性好。     

用HPLC法测定参维冻干蜂王浆片中维生素B1和维生素B2含量

目的 建立参维冻干蜂王浆片中维生素B1和维生素B2的含量测定方法.方法 用KANTO CHEMICAL Co.,Inc,Mightysil C18色谱柱(250×4.6 mm,5μm),以乙腈-0.032%的辛烷基磺酸钠溶液(取辛烷基磺酸钠0.32g,加冰醋酸3ml和三乙胺3ml,加水溶解至1000ml)(10∶90)为流动相,流速1.0ml·min-1,检测波长为270nm,柱温为35℃.结果 维生素B1的线性范围为16μg·ml-1～800μg·ml-1(r=0.9999),平均回收率为99.4%,RSD=0.9%(n=9);维生素B2的线性范围为2μg·ml-1～104μg·ml-1(r=1.0000),平均回收率为99.6%,RSD=0.7%(n=9).结论 HPLC法适用于参维冻干蜂王浆片中维生素B1和维生素B2的含量测定.     

HPLC法测定复方硫酸锌滴眼液中盐酸小檗碱和尼泊金乙酯的含量

目的:用HPLC法测定复方硫酸锌滴眼液中盐酸小檗碱和尼泊金乙酯的含量.方法:采用Symmetry Shield RP C18色谱柱(250mm×4.6mm,5μm);以0.033mol·L-1磷酸二氢钾(KH2PO4)溶液-乙腈(60:40)为流动相,检测波长256nm.结果:盐酸小檗碱和尼泊金乙酯在线性范围分别为6.3～37.6μg·ml-1(r=0.9999)和1.9～11.3μg·ml-1(r=0.9999),平均回收率分别为99.9%(RSD=0.7%)和99.3%(RSD=1.2%).结论:本方法简便、准确,可用于该制剂中盐酸小檗碱和尼泊金乙酯的含量测定.     

HPLC测定感康片中对乙酰氨基酚、咖啡因和扑尔敏的含量

目的 建立同时测定感康片中对乙酰氨基酚、咖啡因和扑尔敏含量的方法.方法 采用HPLC法.Kromasil-C18柱(150 mm×4.6 mm,5 μm),乙腈-0.05 mol·L-1磷酸二氢钾溶液-三乙胺(10:90:0.2)为流动相,流速1.0 ml·min-1,检测波长222 nm.结果 对乙酰氨基酚的线性范围为120.0～320.0 μg·ml-1(r=0.9998),咖啡因的线性范围为7.2～19.2 μg·ml-1(r=0.9999),扑尔敏的线性范围为0.96～2.56 μg·ml-1(r=0.9999).平均回收率分别为99.4%、100%、99.1%(n=6).结论 所建方法可同时分离3种成分,分离效果好,灵敏度高,重复性好,准确可靠.     

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.     

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.     

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.