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。     

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.     

复合氨基酸胶囊中水溶性维生素的含量测定

目的:建立复合氨基酸胶囊中5种水溶性维生素的含量测定方法.方法:采用高效液相色谱法,用乙腈与庚烷磺酸钠-磷酸钠的水溶液(pH=3.0)为流动相,流速1.0ml·min-1,色谱柱为C18(4.6×250mm,5μm),柱温40℃,检测波长为280nm,进样量为20μl.结果:维生素Bl、维生素B2、维生素B6、维生素C和烟酰胺分别在24.7～75.2μg·ml-1、15.0～44.9μg·ml-1、12.2～37.5μg·ml-1、99.2～299.9μg·ml-1和100.3～300.9μg·ml-1范围内呈线性关系,相关系数均为1.000,平均回收率均在100%±2%范围以内.RSD分别为0.19%、0.26%、0.46%、1.17%和0.52%.结论:本方法准确,简便,快捷,可以同时测定复合氨基酸胶囊中维生素B1、维生素B2、维生素B6、维生素C和烟酰胺的含量.     

珍菊降压片含量及均匀度测定方法研究

目的:建立一种高效液相色谱法测定珍菊降压片中盐酸可乐定的含量及均匀度。方法:采用Diamonsil(钻石)C18(200×4.6mm,5μm)色谱柱;0.05mol/L磷酸二氢钾-乙腈(80:20)为流动相;柱温35℃;流速1.0ml·min-1;检测波长210nm。结果:盐酸可乐定在1.041μg·ml-1～8.328μg·ml-1浓度范围内具有良好的线性关系,R=1.00000;平均回收率为99.99%,RSD(%)=0.68%。结论:该方法准确,可靠,重复性好,可作为珍菊降压片质量控制方法。     

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法同时测定扑麻滴鼻液中2成分的含量

目的:建立同时测定扑麻滴鼻液中盐酸麻黄碱和马来酸氯苯那敏含量的HPLC方法。方法:采用:PurospherSTAR RP18色谱柱(150 mm×4.6 mm,5μm),以磷酸盐缓冲液(p H 3.0±0.1)-乙腈(82∶18)为流动相,流速为1.0 ml·min-1,在210nm波长处同时检测盐酸麻黄碱和马来酸氯苯那敏,柱温35℃,进样量20μl。结果:盐酸麻黄碱和马来酸氯苯那敏分别在19.81~118.85μg·ml-1和6.21~37.25μg·ml-1浓度范围内线性关系良好,r分别为0.999 6和0.999 8。平均回收率分别为100.39%(RSD=0.69%,n=9)和100.11%(RSD=0.60%,n=9)。结论:该方法快速简便、重复性、准确性好,可用于该制剂中盐酸麻黄碱和马来酸氯苯那敏的含量测定。     

HPLC测定7种党参类植物中的党参炔苷

目的 建立测定7种党参中党参炔苷含量的方法.方法 采用RP-HPLC法,色谱柱为依利特C18(250 mm×4.6 mm,5 μm)柱,流动相为乙腈-水(20:80),检测波长为270 nm.结果 党参炔苷的线性范围为0.025～6.180 μg·ml-1(r=0.9999);最低检测限为0.506 μg·ml-1;平均回收率为98.74%,RSD=0.53%(n=6).应用此法测定了7种党参属植物共26个样品中党参炔苷的含量.结论 所建方法快速简便,重复性好,可评价党参类药材的质量.     

高效液相色谱法同时测定小儿感冒冲剂中对乙酰氨基酚和咖啡因的含量

目的:建立同时测定小儿速效感冒冲剂中对乙酰氨基酚和咖啡因含量的高效液相色谱方法.方法:采用HypersilODS C18柱(5μm,250 mm×4.6 mm),流动相为甲醇∶水(30∶70),检测波长为280 nm,峰面积外标法.结果:对乙酰氨基酚在10.08～100.80μg·ml-1,咖啡因在0.592～5.920μg·ml-1浓度范围内线性关系良好;对乙酰氨基酚回收率为98.9%,RSD为0.58%(n=6),咖啡因回收率为100.15%,RSD为2.52%(n=6).结论:该方法具有操作简便、结果准确等优点.     

HPLC法测定妇炎清泡腾片中苦参碱的含量

目的:建立测定妇炎清泡腾片中苦参碱含量的 HPLC 方法。方法:色谱柱为 Diamonsil C_(18)(250 mm×4.6 mm,5μm);流动相为乙腈-0.2%磷酸溶液(30:70,以三乙胺调节至 pH 8.0);流速:1.0 mL·min~(-1);检测波长为220 nm。结果:苦参碱在0.16496～8.248μg之间呈良好线性(r=0.9996),测定样品平均回收率为99.5%,RSD 为0.9%(n=6),3批样品平均含量为3,602 g·片~(-1)。结论:本方法简单、易行,精密度高、重复性好,可用于妇炎清泡腾片中苦参碱的含量测定。     

RP-HPLC法测定氯霉素滴眼液中氯霉素及二醇物的含量

目的:测定氯霉素滴眼液中氯霉素和二醇物的含量.方法:采用RP-HPLC法.色谱系统:色谱柱:Kromasil ODS-1(250×4.6mm)流动相为水-甲醇-冰醋酸(55:45:0.1)[1],流速约为1ml·min-1,检测波长为278nm.结果:氯霉素与二醇物的平均回收率分别为100.6%、100.8%,RSD值分别为0.23%、1.49%.氟霉素线性范围为12.5μg·ml-1～300μg·ml-1,二醇物线性范围为1μg·ml-1～24μg·ml-1.结论:该法快速,简单,准确.可作为该制剂的质量控制标准.     

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.     

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.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

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.     

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.