RP-HPLC法测定PAC-1盐酸盐的含量及有关物质

目的建立RP-HPLC方法测定PAC-1盐酸盐含量并进行有关物质检查。方法采用KromasilC18色谱柱(150 mm×4.6 mm,5μm),流动相:乙腈-甲醇-磷酸盐缓冲液(30 mmo.lL-1磷酸二氢钾,体积分数为0.06%的磷酸溶液)(体积比为35∶5∶60),流速:1.0 mL.min-1,UV检测波长:281 nm,柱温:35℃。结果PAC-1盐酸盐在2.00~50.10 mg.L-1内线性关系良好(r=0.999 9),平均回收率为100.3%(RSD=0.8%)。PAC-1盐酸盐与其有关物质得到良好分离,检测限为0.2 ng。结论本方法可用作PAC-1盐酸盐含量测定和有关物质检查。     

HPLC法测定盐酸法舒地尔的含量及有关物质

目的建立盐酸法舒地尔含量及有关物质的高效液相色谱测定方法。方法采用高效液相色谱法。色谱柱为Agela C18;流动相:0.05mol.L-1的磷酸二氢铵溶液-甲醇(75∶25);检测波长:275nm;柱温:25℃;流速:1.0mL.min-1。结果盐酸法舒地尔在7.5～120μg.mL-1浓度范围内线性关系良好(r=0.9998),平均回收率为99.9%,RSD为0.2%,供试品溶液在24h内稳定。结论该方法简便、准确、可靠,专属性强,可以用于盐酸法舒地尔的含量及有关物质测定。     

Determination of related substance and content in Ranolazine - sustained release tablets by HPLC

目的 采用HPLC测定雷诺嗪缓释片的含量和有关物质.方法 采用Inertsil C18色谱柱(250 mm×4,6 mm,5μm),流动相为乙腈-0.02 mol·L-1磷酸二氢钾-三乙胺(52∶48∶0.1),流速1.0 mL·min-1,检测波长230 nm.结果 雷诺嗪与中间体Ⅰ及其降解产物能有效分离,雷诺嗪20.24～ 506.00 μg· mL -与峰面积线性关系良好(r =0.9999,n=5),平均回收率为99.89％ (RSD =0.61％,n=9),检测限为0.5 ng,中间体Ⅰ对雷诺嗪的相对保留时间约为0.25,相对响应因子约为1.25.结论 所用方法简便、准确、重复性、专属性及灵敏度好,可用于雷诺嗪缓释片中有关物质和含量的测定.     

HPLC整体柱测定利福平注射液的含量及有关物质

目的建立一种更快速灵敏可重现的使用整体柱测定利福平注射液含量和有关物质的HPLC法。方法色谱柱:Chromolith performance RP-18e(100 mm×4.6 mm,流动相:[乙腈-0.075 mol.L-1磷酸二氢钾溶液-1.0 mol.L-1枸橼酸溶液-四氢呋喃(体积比为40∶90∶10∶3)]-甲醇(体积比为3∶2),流速:2.0 mL.min-1,检测波长:254 nm。结果在选定色谱条件下,有关物质与主药分离良好,利福平在6~240 mg.L-1内质量浓度与峰面积呈良好的线性关系,r=0.999 8,平均回收率为100.0%(n=9)。结论该方法可用于利福平注射液中利福平的含量及有关物质的测定。     

HPLC测定硫唑嘌呤中有关物质

目的建立用HPLC测定硫唑嘌呤中有关物质的测定方法。方法采用Phenomenex C18(4.6mm×200mm,5μm)色谱柱,流动相为甲醇-0.05%醋酸钠水溶液(18∶82),流速:1.2mL·min-1,检测波长240nm。结果在选定的色谱条件下,硫唑嘌呤与起始物料、中间体等有关物质完全分离;巯嘌呤在0.45～1.125μg·mL-1(r=0.9999),1-甲基-4-硝基-5-氯咪唑(硝化物)在0.3～0.75μg·mL-1(r=0.9999)内呈良好的线性关系;巯嘌呤和1-甲基-4-硝基-5-氯咪唑平均回收率(n=9)分别为100.1%和99.7%;检测限分别为3ng.mL-1和2ng·mL-1。结论本测定方法简便、准确、专属性好,可用于硫唑嘌呤的有关物质的测定。     

HPLC测定甲钴胺的含量及其有关物质

目的 采用HPLC法测定甲钴胺的含量和有关物质.方法 色谱柱为Kromasil C18柱(250 mm×4.6 mm,5μm),流动相为0.03 mol∶ L-1磷酸二氢钾溶液(用0.2 mol·L-1氢氧化钠或磷酸调pH4.5)-乙腈(84∶16),含量测定和有关物质的检测波长分别为266、342 nm.流速为1.0 mL·min-1.结果 甲钴胺峰的分离度良好,最低检测限为0.18 ng,甲钴胺的线性范围为3.94 ～ 5.92 μg∶ mL-1(r2=0.9999,n=5)和4.93 ～ 78.90 μg· mL-1(r2 =0.9994,n=5).结论 所用方法简便、准确、重复性好,可用于甲钴胺的含量和有关物质的测定.     

HPLC法测定非布司他的含量及有关物质

目的建立测定非布司他原料药含量和有关物质的HPLC方法。方法采用Diamond ODS-C18色谱柱(200 mm×4.6 mm,5μm),流动相为甲醇-乙腈-质量分数为0.05%的磷酸溶液(体积比为24∶46∶30),流速为1.0 mL.min-1,UV检测波长为315 nm,柱温为35℃。结果非布司他在15.7~94.3 mg.L-1内线性关系良好(r=0.999 8),平均回收率为100.5%(RSD=1.0%)。非布司他和其有关物质得到良好分离,检测限为0.5 ng。结论 HPLC法可用于非布司他含量测定和有关物质检测。     

HPLC测定雷诺嗪缓释片的含量及有关物质

目的采用HPLC测定雷诺嗪缓释片的含量和有关物质。方法采用Inertsil C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.02 mol·L-1磷酸二氢钾-三乙胺(52∶48∶0.1),流速1.0 mL·min-1,检测波长230 nm。结果雷诺嗪与中间体Ⅰ及其降解产物能有效分离,雷诺嗪20.24～506.00μg·mL-1与峰面积线性关系良好(r=0.9999,n=5),平均回收率为99.89%(RSD=0.61%,n=9),检测限为0.5 ng,中间体Ⅰ对雷诺嗪的相对保留时间约为0.25,相对响应因子约为1.25。结论所用方法简便、准确、重复性、专属性及灵敏度好,可用于雷诺嗪缓释片中有关物质和含量的测定。     

HPLC法测定中间体7-TACA含量和有关物质

目的 建立有效、简便、快速的高效液相色谱法测定中间体7-氨基-3-(1,2,3-三唑-4-硫代)甲基-头孢环-4-羧酸(7-TACA)的含量和有关物质;方法 色谱柱:C18色谱柱,流动相:0.03 mol/L磷酸二氢钾溶液-乙腈(95∶5),流速为1.0mL/min,检测波长272 nm,柱温35℃,进样量20 μL;结果 7-TACA在1.00～794.00μg/mL浓度范围内与峰面积呈良好的线性关系,Y=4×107X-53694,n=8,相关系数r=0.9999.最低检出浓度为0.6 ng/mL,最小定量浓度为0.6 ng/mL.结论 该方法为中间体7-TACA含量测定和有关物质检查提供了方便、灵敏、精确、可靠的方法.为成品的质量提供了保证.     

反相离子对色谱法测定α-酮亮氨酸钙的含量及有关物质

目的建立测定α-酮亮氨酸钙原料药含量和有关物质的反相离子对色谱方法。方法采用Diamond ODS-C18色谱柱(250 mm×4.6 mm,5μm),流动相:乙腈-0.05 mo.lL-1磷酸二氢钾缓冲液(pH2.5)(体积比为23∶67),内含质量分数为0.1%的氢氧化四丁基铵,流速:1.0 mL.min-1,紫外检测波长:220 nm,柱温:30℃。结果α-酮亮氨酸钙在40~160 mg.L-1内线性关系良好(r=0.999 7),平均回收率为100.4%(RSD=0.71%)。α-酮亮氨酸钙和其有关物质得到良好分离,检测限为16 ng。结论本方法可用于α-酮亮氨酸钙含量测定和有关物质检查。     

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.