HPLC-PDA法同时测定更年宁中芍药苷、阿魏酸、黄芩苷和丹皮酚的含量

目的建立HPLC-PDA法同时测定更年宁中芍药苷、阿魏酸、黄芩苷和丹皮酚的含量。方法采用Phenomsil C18(4.6 mm×250 mm,5μm)色谱柱;流动相:以乙腈为流动相A,以0.15%磷酸为流动相B,采用梯度洗脱;流速为1.0 mL·min~(-1);柱温为35℃;芍药苷的检测波长为230 nm,阿魏酸的检测波长为320 nm,黄芩苷的检测波长为280 nm,丹皮酚的检测波长为274 nm。结果芍药苷、阿魏酸、黄芩苷、丹皮酚浓度分别在5.077～50.77、0.297～2.97、8.976～89.76、3.37～33.70μg·mL~(-1)与峰面积线性关系良好,平均回收率分别为98.5%(RSD=0.83%)、98.4%(RSD=1.5%)、98.9%(RSD=1.1%)、98.4%(RSD=1.0%)。结论该方法简便、灵敏、结果准确可靠,可为其提高质量控制标准提供参考。     

HPLC法同时测定女金胶囊中黄芩苷和丹皮酚的含量

目的:高效液相色谱法测定女金胶囊中黄芩苷和丹皮酚的含量.方法:色谱柱:Symmetry C18柱(150 mm×3.9 mm,5μm);流动相:甲醇-0.4％磷酸(48∶52),流速:1ml ·min-1;紫外检测波长:276 nm;柱温:30℃;进样量:10μl.结果:在4.96～24.80 μg和2.60～13.00 μg范围内成线性关系,平均回收率分别为98.3％和98.4％(n=6).结论:该方法简便,准确,可作为女金胶囊中黄芩苷和丹皮酚含量的测定方法.     

高效液相色谱法同时测定安坤胶囊中栀子苷、芍药苷、特女贞苷、蟛蜞菊内酯和丹皮酚的含量

目的建立HPLC法同时测定安坤胶囊中栀子苷、芍药苷、特女贞苷、蟛蜞菊内酯和丹皮酚含量。方法采用Agilent TC-C18色谱柱(4.6 mm×250 mm,5μm),流动相:乙腈-0.1%磷酸水溶液,梯度洗脱;检测波长230 nm(0～30 min)、351 nm(30～40 min)、274 nm(40～50 min);流速1.0mL·min~(-1);柱温30℃,进样量:10μL。结果栀子苷、芍药苷、特女贞苷、蟛蜞菊内酯和丹皮酚分别在81.83～4091.69 ng(r=0.9999)、79.71～3985.61 ng(r=0.9999)、15.58～778.91 ng(r=0.9999)、1.35～67.40 ng(r=0.9992)、16.54～827.20 ng(r=0.9998)与峰面积线性关系良好;平均回收率分别为98.5%、97.2%、97.9%、102.9%、97.6%,RSD值分别为0.80%、1.0%、1.6%、2.6%、1.9%。结论该方法简便、快速、重复性好,可用于安坤胶囊的质量控制。     

超高效液相色谱法同时测定白芍中芍药苷和芍药内酯苷的含量

目的 采用超高效液相色谱法(UPLC)同时测定白芍中芍药苷和芍药内酯苷的含量.方法 采用Agilent Extend-C18(4.6 mm×50 mm,1.8μm)色谱柱,以流动相乙腈(A)-0.2％乙酸溶液(B)梯度洗脱;柱温30℃;流速0.5 mL·min-1;检测波长230 nm.结果 芍药苷和芍药内酯苷分别在0.011 6～1.45(r=0.999 9)、0.008～lmg·mL-1(r=0.999 9)呈良好的线性关系;平均回收率分别为98.6％、97.5％,RSD分别为1.4％、2.2％.结论 该法快速简便,灵敏度高,准确可靠,可用于白芍中有效成分含量的快速测定及白芍的质量控制.     

超高效液相色谱法同时测定丹蛭降糖胶囊中丹皮酚和芍药苷含量

目的:建立一种超高效液相色谱法同时测定丹蛭降糖胶囊中丹皮酚、芍药苷的含量。方法:色谱柱为Waters Acquity UPLC BEH C18(50 mm×2.1 mm,1.7μm)柱,以乙腈-0.1%磷酸为流动相进行梯度洗脱,流速为0.25 mL.min-1,柱温为30℃,检测波长为230 nm。结果:丹皮酚和芍药苷的线性范围分别为0.653～1.959μg(r=0.999 7)和0.108～0.324μg(r=0.999 9),平均加样回收率分别为99.46%,RSD=0.46%(n=6)和99.19%,RSD=0.49%(n=6)。结论:新建方法简便、快速、准确、易行,可用于控制制剂质量。     

HPLC法双波长同时测定赤芍中4种成分的含量

目的：采用高效液相色谱法,在不同检测波长下同时测定赤芍中儿茶素、芍药苷、苯甲酸、丹皮酚4种成分的含量。方法色谱柱为DiamonsilC185μm250＆#215;4.6mm,以0.1%甲酸-乙腈为流动相进行梯度洗脱,检测波长为230nm（儿茶素、芍药苷、苯甲酸）,275nm（丹皮酚）,流速1mL·min-1,柱温30℃。结果不同产地赤芍中4种成分含量差异较大,7批不同产地赤芍药材中儿茶素、芍药苷、苯甲酸和丹皮酚的含量范围分别为：0%-0.052%、1.044%-4.326%、0.126%-0.249%、0.022%-1.060%。结论本法操作简便、准确、重复性好,可用于赤芍药材中儿茶素、芍药苷、苯甲酸、丹皮酚含量的测定。     

六味地黄丸中四种活性成分的HPLC法测定

建立了HPLC法同时测定六味地黄丸中的丹皮酚、马钱苷、莫诺苷和芍药苷.采用C_(18)色谱柱,以乙腈-0.1%磷酸溶液梯度洗脱,检测波长238 nm,丹皮酚、马钱苷、莫诺苷和芍药苷分别在0.5～20、0.25～10、0.5～20和0.15～6μg/ml浓度范围内线性关系良好,回收率分别为98.10%～105.44%.     

HPLC波长切换法同时测定白芍饮片中9个成分的含量

目的:建立高效液相色谱波长切换法对白芍中9个成分(没食子酸、氧化芍药苷、儿茶素、芍药内酯苷、芍药苷、苯甲酸、1,2,3,4,6-五没食子酰葡萄糖、苯甲酰芍药苷、丹皮酚)进行分析。方法:采用Phenomsil ODS(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-0.1%磷酸水(B)为流动相,梯度洗脱,流速1.0 mL.min-1,检测波长为267 nm(0～12 min,测定没食子酸)、258 nm(12～30 min,测定氧化芍药苷、儿茶素)、230 nm(30～38 min,测定芍药内酯苷、芍药苷)、223 nm(38～42 min,测定苯甲酸)、275 nm(42～56 min,测定1,2,3,4,6-五没食子酰葡萄糖)、230 nm(56～70 min,测定苯甲酰芍药苷、丹皮酚)。结果:白芍中9个成分没食子酸、氧化芍药苷、儿茶素、芍药内酯苷、芍药苷、苯甲酸、1,2,3,4,6-五没食子酰葡萄糖、苯甲酰芍药苷、丹皮酚进样量分别在0.13～0.87μg(r=0.9991),0.13～0.85μg(r=0.9991),2.50×10-3～17.50×10-3μg(r=0.9993),0.26～1...     

HPLC-MS/MS法同时测定脑血疏口服液中三种成分的含量

目的采用HPLC-MS/MS法同时测定脑血疏口服液中3种有效成分-芍药苷、黄芪甲苷及丹皮酚的含量。方法选用Phenomenex Luna C_(18)(100 mm×4.6 mm,5μm)色谱柱;以含10 mmol/mL乙酸铵乙腈溶液(A)、10 mmol/mL乙酸铵水溶液(B)为流动相,梯度洗脱;质谱为ESI源负离子-MRM模式下检测,流速为0.3mL/min;柱温为25℃。结果芍药苷、黄芩甲苷及丹皮酚3种成分线性范围分别为0.20~2.00μg(r=0.9991)、2.00~20.00μg(r=0.999 0)、1.00~10.00μg(r=0.998 5),3种化合物的平均回收率分别为100.1%、97.9%、102.3%。结论本方法简便、快捷,重现性好,适用于同时测定脑血疏口服液中芍药苷、黄芪甲苷及丹皮酚的含量。     

HPLC法同时测定桂枝茯苓胶囊中丹皮酚、芍药苷和苦杏仁苷的含量

目的：建立HPLC法同时测定桂枝茯苓胶囊中丹皮酚、芍药苷和苦杏仁苷的含量。方法：采用HPLC法测定桂枝茯苓胶囊中丹皮酚、芍药苷和苦杏仁苷的含量。采用C18柱,流动相为甲醇∶水（55∶45）洗脱,流速为1.0ml·min-1,检测波长为274nm,柱温为30℃,进样体积为10μL。结果：线性范围分别为0.198～3.166μg（r=0.9998）、0.195～3.128μg（r=0.9996）、0.197～30158（r=0.9997）。平均加样回收率分别为99.81%（RSD=2.48%）、99.69%（RSD=1.47%）、99.79%（RSD=2.12%）。结论：本研究建立的方法简便,结果稳定可靠,可用于桂枝茯苓胶囊的质量控制。     

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.     

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.     

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.

     

Lung disease and PKCs

The lung offers a rich opportunity for development of therapeutic strategies focused on isozymes of protein kinase C (PKCs). PKCs are important in many cellular responses in the lung, and existing therapies for pulmonary disorders are inadequate. The lung poses unique challenges as it interfaces with air and blood, contains a pulmonary and systemic circulation, and consists of many cell types. Key structures are bronchial and pulmonary vessels, branching airways, and distal air sacs defined by alveolar walls containing capillaries and interstitial space. The cellular composition of each vessel, airway, and alveolar wall is heterogeneous. Injurious environmental stimuli signal through PKCs and cause a variety of disorders. Edema formation and pulmonary hypertension (PHTN) result from derangements in endothelial, smooth muscle (SM), and/or adventitial fibroblast cell phenotype. Asthma, chronic obstructive pulmonary disease (COPD), and lung cancer are characterized by distinctive pathological changes in airway epithelial, SM, and mucous-generating cells. Acute and chronic pneumonitis and fibrosis occur in the alveolar space and interstitium with type 2 pneumocytes and interstitial fibroblasts/myofibroblasts playing a prominent role. At each site, inflammatory, immune, and vascular progenitor cells contribute to the injury and repair process. Many strategies have been used to investigate PKCs in lung injury. Isolated organ preparations and whole animal studies are powerful approaches especially when genetically engineered mice are used. More analysis of PKC isozymes in normal and diseased human lung tissue and cells is needed to complement this work. Since opposing or counter-regulatory effects of selected PKCs in the same cell or tissue have been found, it may be desirable to target more than one PKC isozyme and potentially in different directions. Because multiple signaling pathways contribute to the key cellular responses important in lung biology, therapeutic strategies targeting PKCs may be more effective if combined with inhibitors of other pathways for additive or synergistic effect. Mechanisms that regulate PKC activity, including phosphorylation and interaction with isozyme-specific binding proteins, are also potential therapeutic targets. Key isotypes of PKC involved in lung pathophysiology are summarized and current and evolving therapeutic approaches to target them are identified.     

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.