高效液相色谱法测定康得灵胶囊中黄芩苷的含量

目的 建立康得灵胶囊中黄芩苷的HPLC测定方法。方法 色谱柱为Agilent Tc-C₁₈色谱柱（4.6 mm×250 mm,5 μm）,柱温为30 ℃;流动相为乙腈-0.5‰磷酸溶液（26：74）,流速为1.0 ml/min,检测波长265 nm。结果 黄芩苷保留时间约为16 min。以峰面积（Y）对进样浓度（X, μg/ml）线性回归,得回归方程：Y=22 114.67 X－112 836.7,r=0.998 8,线性范围5.410~108.2 μg/ml。平均加样回收率为98.78%,RSD为0.74%。结论 本方法操作简便,测定结果准确可靠,可用于康得灵胶囊中黄芩苷的含量测定。     

高效液相色谱法测定壮骨颗粒中补骨脂素与异补骨脂素的含量

目的 建立高效液相色谱法测定壮骨颗粒中补骨脂素和异补骨脂素的含量。方法 色谱柱为Agilent Zorbax C₁₈柱（4.6 mm×250 mm,5 μm）,流动相为甲醇-水（45：55）,检测波长为245 nm,流速为1.0 ml/min,柱温为25 ℃,进样量为10 μl。采用70%乙醇水浴方法提取壮骨颗粒中的补骨脂素和异补骨脂素。结果 补骨脂素与异补骨脂素在3.75~40 μg/ml范围内呈良好的线性关系,对方法精密度（n=6）、重复性（n=6）和稳定性（12 h）进行考察,相对标准偏差（RSD）均小于2%。加样回收率（n=6）为94%~105%。结论 该测定方法简便、快速、准确,可用于壮骨颗粒的临床快速质量控制。     

高效液相色谱法测定乐肤口服液中苦参碱的含量

目的 建立HPLC法测定乐肤口服液中苦参碱含量的方法。方法 色谱柱为Diamonsil Platisil NH₂柱（4.6 mm×250 mm, 5 μm）,流动相为乙腈-异丙醇-3%磷酸水溶液（84：4：12）;流速为1.2 ml/min;进样量5 μl;检测波长205 nm。结果 苦参碱在54.50~872.00 μg/ml浓度范围内线性关系良好,r=0.999 1;平均回收率为99.82%, RSD=1.12%。结论 该法简便、稳定可靠、重复性好,为控制乐肤口服液的质量标准提供了可借鉴的依据。     

高效液相色谱法测定鼻炎灵胶囊中黄芩苷含量

目的 建立高效液相色谱法测定鼻炎灵胶囊中黄芩苷的含量。方法 色谱柱为Waters XBridge C₁₈柱（4.6 mm×250 mm,5 μm）,流动相为乙腈-0.8%甲酸（25：75）,检测波长276 nm,流速1.0 ml/min,柱温30℃,进样量10 μl。结果 黄芩苷在1.25~40 μg/ml范围内（r=0.999 9）呈良好的线性关系,精密度实验中RSD均小于2%,加样回收率在95%~100%之间。结论 该测定方法简便、准确,分离效果好,可用于鼻炎灵胶囊的质量控制。     

清热败毒颗粒剂的质量标准研究

目的 建立清热败毒颗粒剂的质量标准。方法 采用薄层色谱法（TLC）鉴别处方中的板蓝根、连翘、紫花地丁和甘草,采用高效液相色谱法（HPLC）测定绿原酸的含量,色谱柱为Agilent ZORBAX SB-C₁₈柱（4.6 mm×250 mm,5 μm）;流动相为乙腈（A）与含0.2%甲酸的水溶液（B）,梯度洗脱：0~12 min,11%~12%A;流速：1.0 ml/min;柱温：30 ℃;检测波长：327 nm;进样量：20 μl。结果 薄层鉴别色谱中特征斑点明显,专属性强。绿原酸在6.19~396.00 μg/ml浓度范围内呈良好线性关系,其回归方程为Y=60.239 4X+9.096 3（r>0.999 9）,回收率为99.66%（RSD=2.82%）。结论 该法简便、稳定可靠、重复性好,为控制清热败毒颗粒的质量标准提供了可借鉴的依据。     

高效液相色谱法测定山楂精降脂片中齐墩果酸和熊果酸含量

目的 建立高效液相色谱法(HPLC)测定山楂精降脂片中齐墩果酸和熊果酸的含量,有效地控制产品质量。 方法 采用Agilent Zorbax SB C₁₈ 柱(250 mm×4.6 mm,5 μm),以甲醇-0.06 mol/L乙酸铵(85:15)为流动相,流速为0.8 ml/min;检测波长为210 nm;柱温为25 ℃。 结果 齐墩果酸和熊果酸分别在0.124~2.48 μg(r=0.999 7)和0.498~9.96 μg(r=0.999 8)范围内与其峰面积呈良好线性关系。测得齐墩果酸平均回收率为96.9%,RSD为1.26%;熊果酸平均回收率为100.4%,RSD为2.6%。 结论 山楂精降脂片质量稳定,质控方法简便、准确,结果可靠、重现性好 。     

高效液相色谱法测定新保肾片中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量

目的 建立新保肾片中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量测定方法,为生产质量提供保障。方法 采用高效液相色谱法测定,色谱柱为Lichrospher-C₁₈柱(250 mm ×4.6 mm,5 μm),流动相为甲醇:0.1%磷酸溶液(7030),流速为1.0 ml/min,柱温为35 ℃,检测波长为254 nm。结果 芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚分别在2.30~18.4 μg/ml(r=1.0)、2.930~23.44 μg/ml(r=1.0)、5.00~40.0 μg/ml(r=1.0)、14.870~118.96 μg/ml (r=0.999 8)、7.410~59.28 μg/ml(r=0.999 9)范围内有良好的线性关系,平均回收率分别为100.16%、102.91%、99.76%、100.32%、100.44%,RSD分别为1.58%、1.27%、1.67%、1.33%、1.03%(n=9)。结论 该方法准确易行,便于质量控制。     

复方生化颗粒的定性鉴别和含量测定研究

目的 提高复方生化颗粒的质量标准。方法 采用薄层色谱（TLC）法对处方中的甘草、丹参进行定性鉴别;采用高效液相色谱（HPLC）法鉴别苦杏仁苷;采用HPLC法测定处方中的丹酚酸B含量,色谱柱为Agilent HC-C₁₈（4.6 mm×250 mm,5 μm）,流动相为乙腈-0.1%磷酸（23：77）,流速为1.0 ml/min,检测波长为286 nm,柱温为30 ℃。结果 TLC斑点清晰,分离度较好,专属性强,阴性对照无干扰;HPLC法定性鉴别更加准确、可靠与客观;丹酚酸B在1.56~49.92 μg/ml范围内浓度与峰面积呈良好的线性关系（r=0.999 9）,平均回收率为100.07%,RSD为1.61%（n=9）。结论 建立的方法准确、可靠,重复性好,可用于复方生化颗粒的质量控制。     

复方颠茄合剂质量标准研究

目的 提高复方颠茄合剂的质量控制标准。方法 采用薄层色谱法（TLC）对复方颠茄合剂中的吗啡进行定性鉴别;采用高效液相色谱法（HPLC）测定复方颠茄合剂中吗啡的含量。以WondaSil C₁₈（4.6 mm×150 mm,5 μm）为色谱柱;A相：0.01 mol/L磷酸二氢钾溶液-0.002 5 mol/L庚烷磺酸钠溶液（含0.1%三乙胺,磷酸调pH至2.5）,B相：乙腈,A∶B=90∶10为流动相;流速：1.0 ml/min;检测波长：220 nm;柱温：30 ℃。结果 在TLC图谱中可检出吗啡的特征斑点。吗啡在0.525~10.5 μg/ml范围内与其峰面积线性关系良好（r=0.999 9）,平均回收率为99.44%,RSD= 0.23%（n=9）。结论 本方法简便准确,专属性强,能够用于复方颠茄合剂的含量测定和质量控制。     

高效液相色谱法测定气管炎颗粒中黄芩苷的含量

目的 建立高效液相色谱法测定气管炎颗粒中黄芩苷的含量。 方法 采用HPLC法,色谱柱:ZORBAX SB-C₁₈柱(4.6 mm×150 mm,5 μm),以甲醇-0.1%磷酸(47:53)为流动相,流速为1 ml/min,检测波长为280 nm。 结果 黄芩苷在6.63~210 μg/ml范围内呈良好线性关系(r=0.999 8,n=6),平均加样回收率为98.16%,RSD为1.89%。 结论 本法简便、灵敏、准确、重复性好,结果可靠,可有效地控制气管炎颗粒的质量。     

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.

     

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.     

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.