RP-HPLC法测定二母安嗽片中的吗啡

目的 建立一种测定二母安嗽片中吗啡的方法。方法 采用反相高效液相色谱法测定二母安嗽片中吗啡的量。色谱柱为phenomenex Luna C₁₈（2）（250 mm×4.6 mm,5 μm）,流动相为乙腈-0.1%磷酸溶液（15：85）（每100 mL 加0.1 g 庚烷磺酸钠）,柱温40 ℃,体积流量1.0 mL/min,检测波长220 nm。结果 吗啡在3.907～97.680 μg/mL 与峰面积积分值呈良好线性关系,平均回收率为96.78%,RSD=0.64%（n=6）。结论 所建立的方法操作简便、测定准确、重复性良好,可用于二母安嗽片的质量控制。     

舒肝丸(浓缩丸)质量标准完善研究

目的 对舒肝丸（浓缩丸）的质量标准进行完善提高。方法 延胡索、厚朴、木香进行薄层色谱鉴别。HPLC同时测定芍药苷、橙皮苷、柚皮苷及新橙皮苷的含量,采用C₁₈色谱柱,乙腈（A）-0.2%磷酸（B）为流动相梯度洗脱（0~40 min,15% A→25% A）,流速为1.0 ml·min^-1;检测波长为230 nm。结果 薄层色谱斑点清晰,分离度好,专属性强,重复性良好。芍药苷、柚皮苷、橙皮苷、新橙皮苷分别在0.023 81~4.762,0.025 65~10.26,0.022 03~2.644 0,0.025 44~5.087 6 μg内线性关系良好,相关系数均为0.999 9;平均回收率分别为102.6%,101.7%,100.5%,102.9%,RSD分别为0.8%,1.2%,2.3%,0.9%。结论 本实验建立的鉴别和含量测定方法为舒肝丸质量标准的修订完善提供了可靠依据。     

骨痛宁胶囊的质量控制研究

目的 建立骨痛宁胶囊的质量控制方法。方法 用薄层色谱（TLC）法鉴别骨痛宁胶囊的主要成分当归、川芎和白芍,用高效液相色谱-蒸发光散射检测（HPLC-ELSD）法测定黄芪甲苷的量,以Diamonsil C₁₈（250 mm×4.6 mm,5 μm）柱为色谱柱,流动相为乙腈-水（34：66）,体积流量为1.0 mL/min,柱温30 ℃;ELSD条件：漂移管温度为105 ℃,高纯氮气体积流量为2.5 L/min。结果 薄层色谱斑点清晰,分离度良好,阴性对照无干扰。黄芪甲苷在1.02～6.12 μg线性关系良好（r=0.999 1）,平均回收率为99.61%,RSD为2.80%。结论 该方法操作简便,结果准确、可靠,重复性好、专属性强,可用于该制剂的质量控制。     

利血丸质量标准的建立

摘 要 目的： 建立利血丸的质量标准。方法: 用TLC法鉴别处方中的青皮、当归、赤芍、泽泻;运用HPLC法测定青皮中的橙皮苷,采用WondaSil C₁₈色谱柱（250 mm×4.6 mm,5 μm）, 乙腈-水-磷酸(20∶80∶0.1）为流动相,流速：1.0 ml·min^-1,柱温：40℃,检测波长：284 nm。结果: 在TLC中可检出青皮、当归、赤芍、泽泻的特征斑点,阴性对照无干扰;橙皮苷在16.560～82.800μg·mL^-1(r=0.999 8)范围内呈良好的线性关系,平均回收率为98.8%（RSD=1.1%, n=6）。结论:该方法准确、可靠,可用于利血丸的质量控制。     

ASE-HPLC测定保和丸中橙皮苷的含量

目的 建立加速溶剂萃取（accelerated solvent extraction,ASE）-高效液相色谱法测定保和丸中橙皮苷含量的方法。方法 利用ASE提取保和丸中橙皮苷,采用HPLC测定保和丸中橙皮苷的含量,选用Kinete×2.6μXB-C₁₈ 100A色谱柱（100 mm×4.6mm,5 μm）,流动相为甲醇-7%醋酸溶液（37：63）,流速0.7 mL·min^-1,柱温40℃,检测波长283 nm。结果 橙皮苷在3.707~74.140 μg·mL^-1内与峰面积呈良好线性关系,平均加样回收率为99.33%,RSD为0.2%。结论 该方法快速、准确,可用于保和丸中橙皮苷含量的测定。     

HPLC法测定尿石通丸中夏佛塔苷和橙皮苷的含量

摘 要 目的： 建立HPLC法分离和测定尿石通丸中夏佛塔苷和橙皮苷的含量。方法: 以Agilent Zobrax SB C₁₈柱（250 mm×4.6 mm,5 μm）为色谱柱,流动相为乙腈 甲醇 0.4%甲酸溶液,梯度洗脱,检测波长为272 nm,流速为1.0 ml·mim^{-1,进样量:10 μl。结果: 夏佛塔苷在0.000 6 ～0.277 2 mg·ml-1范围内线性关系良好（r=1.000 0）;橙皮苷在0.002 1～0.856 8 mg·ml-1范围内线性关系良好（r=1.000 0）。夏佛塔苷平均回收率为101.83%,RSD=0.27%,橙皮苷平均回收率为98.35%,RSD=0.41%(n=6)。结论: 本方法可用于测定尿石通丸中夏佛塔苷和橙皮苷的含量。}     

HPLC法测定山楂红曲胶囊中洛伐他汀

目的 建立山楂红曲胶囊中洛伐他汀的处理及含量测定方法。方法 色谱柱为Kromasil C₁₈柱（250 mm×4.6 mm,5μm）,紫外检测波长238 nm,柱温25℃,体积流量1.0 mL/min,流动相为甲醇：0.1%磷酸溶液（75：25）。结果 洛伐他汀质量浓度在2.04~306 μg/mL与峰面积线性关系良好,平均回收率为98.58%,RSD=1.12%（n=9）。结论 该方法准确、简便,可用于山楂红曲胶囊的质量控制。     

高效液相色谱法测定苍辛滴鼻剂中绿原酸及木兰脂素的含量

目的 运用高效液相色谱法对苍耳子中的绿原酸及辛夷中的木兰脂素进行含量测定。方法 绿原酸采用高效液相色谱法,色谱柱为Shim-Pack CLC ODS C18柱（250×4.6 mm,5 μm）;乙腈-0.4%磷酸溶液（10∶90）为流动相;检测波长为327 nm;流速：1.0 mL/min。木兰脂素的色谱条件为：用辛基键合硅胶为填充剂Hypersil C8柱（250×4.6 mm,5 μm）为色谱柱;乙腈-四氢呋喃-水（35∶1∶64）为流动相;检测波长为278 nm;流速：1.0 mL/min。结果 绿原酸在12.99～129.90 μg/mL（r=0.999 9）范围内及木兰脂素在19.67～196.70 μg/mL（r=0.999 9）范围内线性关系良好,绿原酸回收率为99.28%,RSD为1.15%（n=9）;木兰脂素回收率为99.42%,RSD为0.68%（n=9）, 3批样品中绿原酸的平均含量为0.818 4、0.818 5、0.818 9 mg/mL;木兰脂素的平均含量为0.163 7、0.163 4、0.164 1 mg/mL。结论 高效液相色谱法简便、灵敏、准确,可作为苍辛滴鼻剂的定量质量控制。     

离子色谱-抑制电导法测定硫酸镁钠钾口服用浓溶液中镁、钠、钾离子

目的 建立离子色谱–抑制电导法同时测定硫酸镁钠钾口服用浓溶液中镁、钠、钾离子的方法。方法 采用Dionex IonPac^TM CS12A色谱柱（250 mm×4 mm）,Dionex IonPac^TM CG12A保护柱（50 mm×4 mm）;以甲烷磺酸溶液为洗脱液,梯度洗脱,体积流量为1.0 mL/min,柱温30 ℃,检测池温度35 ℃,电导检测器,抑制器为Dionex CDRS 600 4 mm,电流值117 mA,进样体积为25 μL。结果 镁在0.72～1.08μg/mL、钠在12.80～19.20 μg/mL、钾在3.20～4.80 μg/mL线性关系良好,平均回收率分别为101.0%、100.7%、102.9%,RSD值分别为1.4%、1.4%、0.7%。结论 该方法简单、快速、准确,能够有效地控制硫酸镁钠钾口服用浓溶液中镁、钠、钾离子。     

清脂胃舒佐餐茶HPLC法指纹图谱的研究及4个成分的含量测定

目的 建立清脂胃舒佐餐茶水溶性成分的高效液相色谱（HPLC）法指纹图谱,并测定没食子酸、绿原酸、柚皮苷、橙皮苷的含量。方法 采用HPLC法,色谱条件：Kromasil C₁₈柱（250 mm×4.6 mm, 5 μm）;流动相为乙腈-0.1%磷酸水溶液,梯度洗脱;流速为0.8 ml/min;检测波长为300 nm;柱温为35℃。结果 通过中药色谱指纹图谱相似度评价系统（2004A）,确定了清脂胃舒佐餐水溶性成分的HPLC指纹图谱共有模式,标定了26个共有峰,整体相识度为0.934~0.995;并测定了10批制剂中绿原酸、柚皮苷、橙皮苷的含量分别为0.672、0.194、1.247和0.532 mg/g,RSD分别为1.35%、1.89%、0.69%和0.79%。结论 清脂胃舒佐餐水溶性成分的HPLC指纹图谱及其中没食子酸、绿原酸、柚皮苷、橙皮苷的含量检测方法简便、稳定、科学,为本品的质量控制提供了科学依据。     

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.     

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.     

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.