银黄颗粒中黄芩苷含量测定方法研究

目的探讨银黄颗粒质量标准.方法采用高效液相色谱法对银黄颗粒中的黄芩苷进行含量测定,色谱柱为Kromasil C18色谱柱(4.6mm×250mm,5μm),以甲醇-水-磷酸(47∶53∶0.2)为流动相;流速:1.0mL.min-1,检测波长274nm.结果黄芩苷的进样量在0.03～0.15mg范围内呈良好的线性关系(r=0.999 5),平均加样回收率为99.99%,RSD为0.07%(n=6).结论方法简便、准确,可用于银黄颗粒中黄芩苷的含量测定.     

HPLC法测定不同厂家银黄颗粒中黄芩苷的含量

目的建立RP—HPLC测定银黄颗粒制剂中黄芩苷含量的方法及测定不同厂家银黄颗粒制剂中黄芩苷的含量。方法采用HPLC法检测银黄颗粒制剂中黄芩苷的含量，色谱条件：Kromasil C18色谱柱，以乙腈-0．4％磷酸水溶液（含0．6％三乙胺，28：72）为流动相，流速1ml／min，检测波长275nm，柱温为室温。结果黄芩苷在0．504～16．128mg／L范围内与峰面积呈良好的线性关系（r=0．99985），平均回收率为97．25％，RSD=2．54％（n=6）。结论本文中所建立的色谱方法可以简便、准确测定银黄颗粒中黄芩苷的含量，重现性较好。各厂家生产的银黄颗粒中黄芩苷含量差别较大，有必要建立黄芩苷的定量控制方法。     

高效液相色谱程序可变波长法测定银黄颗粒中绿原酸和黄芩苷的含量

目的:测定银黄颗粒中绿原酸、黄芩苷的含量。方法:利用二极管阵列检测器的程序可变波长功能,在绿原酸、黄芩苷的最大吸收波长(λmax)同时测定银黄颗粒中绿原酸、黄芩苷含量。HiQsilC18色谱柱;柱温为30℃;流动相为甲醇(A)-0.2%磷酸(B);流速为1mL.min-1;梯度洗脱,0～5min,40%A;5～15min,40%A线性增加至80%A;15min后,80%A;检测波长程序设置为0～5min,327nm(绿原酸);5～15min,280nm(黄芩苷)。结果:绿原酸进样量在0.072～0.72μg范围内线性关系良好(r=0.9999),黄芩苷进样量在0.91～9.1μg范围内线性关系良好(r=0.9999),绿原酸、黄芩苷平均加样回收率为98.0%,97.6%,RSD分别为1.43%,1.87%。结论:该方法简便、准确,具有较好的重复性,可作为银黄颗粒制剂的质量控制方法。     

HPLC同时测定银黄颗粒中绿原酸和黄芩苷的含量

目的建立同时测定银黄颗粒中绿原酸和黄芩苷含量的高效液相色谱方法。方法Agilent Eclipse XDB-C18色谱柱（4.6mm×150mm,5μm）;柱温为30℃;流动相为0.1%磷酸（A）-乙腈（B）;流速为1.0mL·min^-1;梯度洗脱;检测波长为327nm。结果绿原酸在0.021～2.1μg内线性关系良好（r=0.9998）;黄芩苷在0.038～3.800μg内线性关系良好（r=0.9996）。绿原酸、黄芩苷平均加样回收率为99.70%,99.06%,RSD分别为0.75%和1.02%。结论所建立的方法简便、准确可以同时测定银黄颗粒中绿原酸和黄芩苷的含量。     

RP-HPLC法同时测定不同厂家银黄颗粒中绿原酸、木犀草苷和黄芩苷的含量

目的建立HPLC法同时测定银黄颗粒中绿原酸、木犀草苷和黄芩苷的方法。方法采用Kromasil C18柱(250 mm×4.6 mm,5μm),乙腈-0.4%磷酸水溶液为流动相的梯度洗脱模式分离各测定组分,采用可变波长的方式测定相应组分的峰面积并计算样品含量。结果绿原酸、木犀草苷和黄芩苷分别在0.020 13～2.013μg(r=0.999 9)、0.004 93～0.493μg(r=0.999 8)及0.057 62～5.762 43μg(r=0.999 9)范围内具有良好的线性关系;且平均加样回收率分别为100.2%,RSD为0.2%(n=6);99.1%,RSD为2.0%(n=6);100.8%,RSD为1.4%(n=6);重复性试验,3个成分含量的RSD均小于2.0%(n=6)。结论所建立的方法简便、快速、准确,具有良好的重复性和稳定性,可用于银黄颗粒的质量控制。     

高效液相色谱法测定银黄颗粒中黄芩苷的含量

目的:建立测定银黄颗粒中黄芩苷含量的方法.方法:高效液相色谱法采用Nucleosil C18柱,流动相乙腈-1%醋酸(26:74),流速为1.2 mL·min-1,检测波长为276 nm.结果:黄芩苷浓度线性范围18～45 mg·L-1,相关系数为0.9996,平均回收率为99.58%,RSD为0.53%(n=6).结论:本法操作简便、准确、重复性好,可作为该制剂的定量分析方法.     

HPLC同时测定银黄颗粒中绿原酸和黄芩苷的含量

目的 建立同时测定银黄颗粒中绿原酸和黄芩苷含量的高效液相色谱方法。方法 Agilent Eclipse XDB-C₁₈色谱柱(4.6 mm ×150 mm, 5 μm);柱温为30 ℃;流动相为0.1%磷酸(A) -乙腈 (B);流速为1. 0 mL·min^-1;梯度洗脱;检测波长为327 nm。 结果 绿原酸在0.021 ~ 2.1 μg内线性关系良好(r=0.999 8);黄芩苷在0.038 ~ 3.800 μg内线性关系良好(r=0.999 6)。绿原酸、黄芩苷平均加样回收率为99.70%,99.06%,RSD分别为0.75%和1.02%。结论 所建立的方法简便、准确可以同时测定银黄颗粒中绿原酸和黄芩苷的含量。     

HPLC法测定银黄片中黄芩苷的含量

目的 建立测定银黄片中黄芩苷的含量测定方法.方法HPLC法,采用Shimadzu C18柱(150 mm× 4.6 mm,5 μm);流动相为甲醇-水-冰醋酸(45:55:1);流速为1.0 ml·min-1.拄温为40 ℃.检测波长为274 nm.结果 黄芩苷在2.072～10.360 μg范围内呈良好线性关系,r=0.9996;平均回收率为97.87%,RSD为0.55%.结论 所建立的方法可准确、快速地测定银黄片中黄芩苷的含量,可用于该制剂的质量控制.     

银黄含片中黄芩苷、绿原酸含量测定方法的研究

目的为银黄含片建立含量测定方法.方法采用HPLC-DAD检测器实现了同时测定银黄含片的绿原酸、黄芩苷含量.结果采用HPLC—DAD同时测定银黄含片的两种主成分——绿原酸、黄芩苷的含量,方法准确度、精密度、灵敏度等指标均符合要求.克服了绿原酸、黄芩苷的相互干扰,结果更能反映制剂的真实含量.结论获得一种能同时测定绿原酸、黄芩苷含量的测定方法,为银黄系列产品的检测提供了依据.     

HPLC测定复方银黄片中黄芩苷的含量

目的建立用HPLC测定复方银黄片中黄芩苷含量的方法。方法用Sh im-pack CLC-ODS 6.0×150 mm柱,甲醇-水-磷酸(50∶50∶0.2)为流动相[1],检测波长为274 nm。结果进样量在7~63μg范围内具有良好的线性关系;黄芩苷的平均回收率为99.7%(n=5),RSD为0.2%。结论该方法快速、方便,能准确检出黄芩苷的含量。     

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.     

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.