HPLC法测定风湿福音丸中马钱子碱、士的宁的含量

目的建立风湿福音丸中马钱子碱、士的宁的含量测定方法。方法采用ApolloC18为分析柱,乙腈-0.01mol·L^-1庚烷磺酸钠与0.02mol·L^-1磷酸二氢钾等量混合溶液（用10%磷酸调节pH值2.8）（20∶80）为流动相;流速为0.8mL·min^-1,检测波长为260nm。结果线性范围：士的宁0.05984～0.8976μg,r=0.99995,平均回收率为100.57%;RSD为2.38%（n=6）。马钱子碱0.04228～0.6342μg,r=0.9994,平均回收率为98.12%;RSD为1.56%（n=6）。结论该法操作简便、准确、分离度与稳定性好、专属性强,可作为控制该制剂的质量方法。     

复方马钱子片中士的宁和马钱子碱含量的测定

目的:建立复方马钱子片中士的宁和马钱子碱的含量测定方法.方法:采用高效液相色谱法,以甲醇 乙腈 水 冰醋酸(35∶40∶25∶0.5)为流动相,ZorbaxSB C18ODS(4.6 mm×250.0 mm,5 μm)为分析柱,紫外检测波长为254 nm.结果:士的宁线性范围为0.05～0.45 μg,r＝0.999 7,测量平均回收率99.4%,RSD 2.2%.马钱子碱线性范围0.06～0.54 μg,r＝0.999 4,测量平均回收率101.3%,RSD 1.22%.结论:高效液相色谱法测定复方马钱子片中士的宁和马钱子碱含量简便、快速、灵敏.     

腰腿痛片质量标准研究

目的建立腰腿痛片质量标准。方法采用薄层色谱法对处方中马钱子、防己、当归进行定性鉴别，用紫外分光光度法测定处方中马钱子中士的宁的含量。结果薄层色谱检出了马钱子、防己、当归的特征斑点；士的宁质量浓度线性范围是2．18-19．64μg／mL，r=0．9998（n=6），平均加样回收率为99．86％，RSD=0．15％（n=6）。结论方法简便准确，重现性好，可用于该制剂的质量控制。     

高效液相色谱法测定蒙药顺气安神丸中马钱子碱和士的宁含量

目的：建立顺气安神丸中马钱子碱和士的宁的含量测定方法.方法：高效液相色谱法,以SHMADZUC18柱和phenomenex C18（均为250minx4.6mm,5μm）为色谱柱,以乙腈-0.02mol/L庚烷磺酸钠与0.04mol/L磷酸二氢钾等量混合溶液（用10%磷酸调节PH值2.8）（18.5：81.5）为流动相,检测波长260nm.结果：马钱子碱进样量在0.0516μg～1.0336μg范围内与峰面积线性关系良好,r=0.9999,平均回收率为99.4%,RSD为0.86%（n=6）;士的宁进样量在0.0906μg～1.8120μg范围内与峰面积线性关系良好,r=0.9999,平均回收率为99.9%,RSD为0.89%（n=6）.结论：该方法灵敏、准确,重复性、专属性好,适用于顺气安神丸中毒性药材马钱子的质量控制.     

HPLC法测定止痛风湿丸中马钱子碱和士的宁的含量

目的建立止痛风湿丸中马钱子碱和士的宁的高效液相色谱的分析法。方法采用lunaC18色谱柱(4.6mm×250mm,5μm);流动相为乙腈-0.01mol/L庚烷磺酸钠与0.02 mol/L磷酸二氢钾等量混合液(用10%磷酸调节pH值至2.8)(22∶78);流速1.0mL/min;检测波长为260nm。结果马钱子碱在0.06608～1.652μg(r=0.99988)、士的宁在0.04064～1.0160μg(r=0.99998),范围内呈良好的线性关系;马钱子碱平均回收率为98.4%,RSD为1.1%;士的宁平均回收率为98.6%,RSD为1.0%。结论本方法准确可靠,简便灵敏,重现性好,可用于止痛风湿丸中马钱子碱和士的宁的质量控制。     

HPLC测定风湿安泰片中马钱子碱和士的宁的含量

目的:采用反相高效液相色谱法测定风湿安泰片中士的宁和马钱子碱的含量。方法:采用 Hypersil BDS C_(18)色谱柱(4.6 mm×250 mm,5 μm),保护柱(4.6 mm×12 mm);乙腈-0.3%三乙胺溶液(磷酸调 pH=2.6)(10:90)为流动相,流速:1.0 mL·min~(-1),柱温:室温,检测波长:254 nm。结果:士的宁在4.6～46μg·mL~(-1)(r=0.9998),马钱子碱在2.65～26.5μg·mL~(-1)(r=0.9998)范围内呈良好的线性关系,士的宁的平均回收率(n=5)为101.1%,RSD 为2.8%;马钱子碱的平均回收率(n=5)为99.6%,RSD 为2.9%。结论:本方法准确、简便、快速,适用于风湿安泰片的质量控制。     

HPLC法测定山药丸中士的宁、马钱子碱的含量

目的：建立测定山药丸中士的宁和马钱子碱含量的方法。方法：采用HPLC法，色谱柱为Luna C18（4.6 mm×250 mm，5μm）；流动相为乙腈-0.0lmol?L-1庚烷磺酸钠与0.02mol?L-1磷酸二氢钾等量混合溶液(用10％磷酸调节pH值至2.8)(21∶79)，流量1.0mL?min-1，柱温35℃，检测波长为260nm。结果：士的宁和马钱子碱的线性范围分别为0.03～0.95μg（r=1.0000）、0.03～1.17μg（r=0.9995），平均回收率(n=6)分别为98.5%、99.0%，其RSD分别为1.4%、0.8%。结论：所建方法可靠、准确，可用于该制剂的质量控制。     

RP—HPLC法测定瘫痿胶囊中马钱子碱和士的宁的含量

目的建立以反相高效液相色谱法测定瘫痿胶囊中马钱子碱和士的宁含量的方法。方法色谱柱为依利特C18（4．6×150mm，5μm），流动相为：0．01mol／L庚烷磺酸钠与0．02mol／L磷酸二氢钾等量混合溶液（用10％磷酸调节pH值2．8）-乙睛（79：21），流速：1．0ml／min，检测波长：260mm，柱温：30℃。结果马钱子碱进样量在0．1296～1．9440μg（r=0．99996）范围内，士的宁的进样量在0．1338—2．0070μg（r=0．99993）的范围内与峰面积积分值呈良好的线性关系。平均加样回收率马钱子碱为99．91％，RSD=1．95％，（n=6）；士的宁为99．60％，RSD=1．48％，（n=6）。结论本方法简便、快速、准确、重现性好，可用于瘫痿胶囊的质量控制。     

反相高效液相色谱法测定痹痛消丸中士的宁和马钱子碱的含量

建立痹痛消丸中士的宁和马钱子碱的反相高效液相分析法。采用Diamonsil C18色谱柱;流动相为乙腈-甲醇-0.05mol.L-1KH2PO4溶液-三乙胺(25∶19∶55∶1),磷酸调pH至3.5;流速1ml.min-1;检测波长254nm。士的宁在15.49~185.88μg.ml-1(r=0.9999)、马钱子碱在5.05~60.60μg.ml-1(r=0.9998)范围内呈良好的线性关系;士的宁平均回收率为98.42%,RSD为1.14%;马钱子碱平均回收率为100.30%,RSD为1.07%。本方法准确可靠,简便灵敏,重现性好,可用于痹痛消丸中士的宁和马钱子碱的质量控制。     

补筋片的质量控制研究

目的建立补筋片质量控制方法。方法采用薄层色谱法鉴别补筋片中丹参、制何首乌;采用高效液相色谱法测定士的宁、马钱子碱含量。结果薄层色谱法可以很好的鉴别丹参、制何首乌;士的宁在0．1338～2．007μg间线性关系良好（r=0．9999）,平均回收率为98．98％（RSD=2．61％）;马钱子碱在0．1296～1．944μg间线性关系良好（r=0．9998）,平均回收率为100％（RSD=2．11％）。结论该法操作简便、准确,可用于该制剂的质量控制。     

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.