血必净注射液指纹图谱研究

目的:建立血必净注射液HPLC指纹图谱及多成分含量测定方法,评价不同批次血必净注射液的质量。方法:HPLC法。采用Agilent Eclipse XDB-C18(250mm×4.6mm,5μm)色谱柱,以乙腈-甲醇-冰醋酸(60∶40∶0.5)-0.5%冰醋酸梯度洗脱,流速1mL·min-1,检测波长280nm,柱温30℃。结果:10批次样品与对照指纹图谱的相似度均大于0.97;同时测定了10批样品中原儿茶醛、羟基红花黄色素A、芍药苷、阿魏酸、洋川芎内酯I及丹酚酸B等6种成分的含量。结论:以指纹图谱相似度评价,不同批次血必净注射液质量基本一致,score分布图相对分散;有些成分含量存在差异。     

RP-HPLC法测定三七总皂苷注射液中9种皂苷的含量

目的建立同时测定三七总皂苷注射液中多种皂苷成分的RP-HPLC法.方法 Zorbax Eclipse XDB-C18色谱柱(250 mm×4.6 mm, 5 μm);乙腈-水梯度洗脱,乙腈:0～30 min,18%→19%;30～35 min,19%→35%;35～60 min,35%→55%.流速1.5 ml·min-1;检测波长203 nm;柱温为40 ℃.结果三七皂苷R1,人参皂苷Rg1、Re、Rf、Rb1、Rc、Rb2 Rb3和Rd的线性范围分别为0.24～4.75 μg(r=0.999 9),0.57～11.40 μg(r=1.000 0),0.50～9.90 μg(r=1.000 0),0.24～4.80 μg(r=1.000 0),0.54～10.65 μg(r=1.000 0),0.26～5.10 μg(r=1.000 0),0.25～4.90μg(r=1.000 0),0.32～6.30 μg(r=1.0000);平均回收率为99.3%～100.2%.结论 RP-HPLC法可同时测定三七总皂苷注射液中9种皂苷含量,有利于其质量控制.     

血必净注射液超高效液相数字化指纹图谱及4种酚酸类化合物含量测定

目的：采用超高效液相色谱法对不同批次血必净注射液进行指纹图谱的建立及特征成分定量分析,建立血必净注射液的质量控制方法。方法：色谱条件采用ACQUITY UPLC^® HSS T3色谱柱（100 mm×2.1 mm,1.8 μm）,以乙腈-0.1%甲酸水为流动相梯度洗脱,流速0.2 mL·min^-1,进样量10 μL,检测波长268.3 nm,柱温40 ℃。对10个批次的血必净注射液进行测定,建立指纹图谱并对其中的4种酚酸类化合物原儿茶酸、原儿茶醛、丹酚酸B、丹酚酸A 进行含量测定。结果：10个批次血必净注射液的指纹图谱相似度均大于0.98,具有良好的相似度,共标定共有峰39个并归属了其中的4个;方法学验证结果表明线性、精密度、重复性、稳定性、加样回收率均符合相关实验要求;血必净注射液中原儿茶酸、原儿茶醛、丹酚酸B、丹酚酸A的平均含量分别为5.26,12.86,2.99,16.37 μg·mL^-1。结论：数字化特征指纹图谱研究并结合主要成分含量测定能够更好、更全面为血必净注射液质量控制提供科学方法和理论基础。     

邻苯二甲醛-9-氯甲酸芴甲酯柱前衍生HPLC法测定血必净注射液中氨基酸

目的通过建立HPLC分析法测定血必净注射液中氨基酸,为提高中药注射液质量标准提供依据.方法通过OPA-FMOC柱前衍生化法,建立同时检测血必净注射液中18种常见氨基酸的液相色谱法.色谱柱为Agilent SB-C18柱(250mm×4.6 mm,5 μm);流动相A为0.02 mol/L醋酸钠溶液(含200μL/L三乙...     

离子色谱法测定中药材中二氧化硫的含量

目的:建立离子色谱法测定中药材中二氧化硫含量的检测方法.方法:采用AS-11-HC色谱柱(250 mm×4 mm,5 μm),保护柱AG-11-HC(50 mm×4 mm,5 μm),以30 mmol·L-1氢氧化钠溶液为淋洗液,甲醛为SO32-的稳定剂,流速为1.0 ml·min-1.结果:硫酸盐标准溶液在5～5 000 ng范围内线性关系良好(r=1.000 0).平均回收率为100.94%(RSD=2.58%,n=15).结论:本法灵敏、准确,简便易行,重复性好,可用于中药材的二氧化硫的含量测定.     

一测多评法测定补骨脂中5种成分的含量

目的建立能测定补骨脂中5种成分含量的一测多评法(QAMS)。方法采用HPLC法,使用Zorbar RRHD SB-C_(18)(150 mm×2.1 mm,1.8μm)和Shim-pack XR-ODSⅢC_(18)(150 mm×2.0 mm,2.2μm)色谱柱,以乙腈-2 mL·L~(-1)冰醋酸为流动相,梯度洗脱;流速:0.4 mL·min~(-1);柱温:45℃;检测波长:246 nm。以补骨脂素为参照物,建立其与异补骨脂素、新补骨脂异黄酮、补骨脂二氢黄酮和补骨脂酚的相对校正因子(RCFs),计算各成分含量,利用外标法与QAMS法测定5种成分的含量,并比较2种方法的含量差异。结果 5种成分的质量浓度分别在3.20～320.23(r_1=0.999 9),2.70～312.91(r_2=0.999 9),2.20～219.45(r_3=1.000 0),2.72～271.76(r_4=1.000 0),1.60～320.68(r_5=0.999 9)μg·mL~(-1)范围内线性关系良好,异补骨脂素、新补骨脂异黄酮、补骨脂二氢黄酮和补骨脂酚相对补骨脂素的RCFs重复性良好,QAMS法的计算结果与外标法测得结果无显著差异。结论 QAMS法能准确测定补骨脂中5种成分的含量,可用于补骨脂中多指标的质量控制。     

半边旗5F注射液中有效成分的含量测定方法

目的:建立半边旗5F(化学名为11α-羟基-15-氧-16-烯-对映贝壳杉烷-19-酸)注射液中有效成分的含量测定方法.方法:采用高效液相色谱法测定主要成分5F的含量,色谱柱为Hypersil C18(250 mm×4.6mm,5μm),流动相为甲醇-水-冰醋酸(55:45:0.045),检测波长为254 nm,流速为1.0 mL·min-1,柱温为35℃.结果:高效液相色谱法测定5F的含量在30～240 mg·L-1范围内线性关系良好(r=0.999 8),平均加样回收率为99.8%.结论:本实验所建立的分析方法灵敏可靠,可作为半边旗5F注射液中有效成分的定量分析方法.     

某院常用中药注射剂与不同溶媒调配后的稳定性研究

目的:考察中国科学技术大学附属第一医院(安徽省立医院)常用中药注射剂参麦、血必净和参附注射液与临床常用溶媒调配后成品输液的稳定性，以期为临床安全合理用药提供技术指导。方法:参照《中国药典》(2020年版)通用技术要求，将参麦、血必净和参附注射液与不同溶媒调配成临床常用浓度的成品输液，分别于0,2,4,6,8,12,24 h时间点取样，考察其成品输液的pH值、渗透压和不溶性微粒数。结果:(1)pH:在0～24 h内，参麦、血必净、参附注射液与不同溶媒调配后成品输液的pH范围在4.03～8.98,接近人体pH(5～8),且随着时间的推移变化不大，成品输液pH变化差值均<1.0。(2)渗透压：在0～24 h内，参麦、血必净、参附注射液与0.9%氯化钠注射液(0.9%sodium chloride injection, 0.9%NS)和5%葡萄糖注射液(5%glucose injection, 5%GS)调配后成品输液的渗透压范围在278～311 mOsmol·kg^-1,接近人体血浆渗透压(280～310 mOsmol·kg^-1),且随着时间的...     

血必净对大鼠肝缺血-再灌注后肾损伤的保护作用

目的 探讨血必净注射液对肝脏缺血-再灌注后肾损伤的保护作用及机制.方法 将90只健康雄性Wistar大鼠随机分为3组:假手术组(SOG组)30只,缺血再灌注组(I/R组)30只,血必净组(XBJ组)30只.血必净组术前3 d经尾静脉注射血必净注射液5ml·kg-1·d-1.于再灌注6 h、12 h、24 h各组分别随机选取10只大鼠进行标本检测:观察动物肾脏组织病理切片;测量肾脏组织中脂质过氧化产物丙二醛(MDA)和超氧化物歧化酶(SOD)的含量.结果 光镜下I/R组、XBJ组与SOG组在相同时相点比较,I/R组病理改变较XBJ组严重; XBJ组与I/R组在相同时相点比较MDA含量显著下降,SOD活性显著升高,差异均有统计学意义(P＜0.01).结论 血必净注射液对肝脏缺血-再灌注后肾损伤具有保护作用,该作用与减少氧自由基的产生有关.     

高效液相色谱法测定复方维生素胶囊中维生素B6与叶酸的含量

目的:建立测定复方维生素胶囊中维生素B6和叶酸含量测定的色谱分析方法.方法:采用Hypersil ODS2色谱柱(4.6 mm× 200mm,5μm);以甲醇-0.05 mol·L-1磷酸二氢钾缓冲液(11:89,pH 5.4)为流动相;流速1.0 mL·min-1;检测波长280 nm处测定.结果:维生素B6与叶酸分别在15.9～142.8mg·L-1,0.372～2.976 mg·L-1范围内呈线性关系;r分别为1.000 0,0.999 8.平均回收率分别为99.95%(RSD为0.83%),100.14%(RSD为1.35%).结论:本法同时测定复方维生素胶囊中维生素B6和叶酸的含量,方法简便、准确.     

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.