高效液相色谱-蒸发光散射测定三七中三七皂苷R1及人参皂苷Rg1、Re、Rb1的含量

目的:用 HPLC—ELSD 测定三七药材中三七皂苷 R_1及人参皂苷 Rg_1、Re、Rb_1的含量。方法:色谱柱为 Lichrospher NH_2柱(4.6 mm×250 mm,5μm),流动相为乙腈-水(80:20);漂移管温度为90℃,载气流速为2.1 L·min~(-1)。结果:三七皂苷 R_1及人参皂苷 Rg_1、Re、Rb_1分别在0.316～1.58μg、1.21～6.05μg、0.448～2.24μg及1.49～7.47μg呈良好线性关系;药材中4种成分的平均回收率(n=6)分别为102.2%(RSD=2.6%)、99.4%(RSD=2.2%)、101.8%(RSD=2.5%)及97.6%(RSD=2.4%)。结论:该方法简便、准确,分离效果好,无干扰,可用于三七药材的质量评价。     

HPLC法测定红药胶囊中三七皂苷R1及人参皂苷Rg1的含量

目的:建立红药胶囊中三七皂苷 R_1及人参皂苷 Rg_1的含量测定方法。方法:采用 Alltima—C_(18)(4.6 mm×150 mm,5μm),流动相为乙腈-0.1%磷酸溶液(20:80),流述为1.0 mL·min~(-1),检测波长为203 nm;柱温为40℃,外标法测定。结果:三七皂苷 R_1和人参皂苷 Rg_1进样量分别在0.345～2.76μg(r=0.9999)和0.945～7.56μg(r=0.9999)范围内与峰面积呈良好线性关系;平均回收率(n=6)分别为98.6%和99.2%。结论:本法简便可靠,专属性强,可用于红药胶囊的质量检测。     

RP—HPLC梯度洗脱法测定血塞通片中三七皂苷R1、人参皂苷Rb1及人参皂苷Rg1的含量

目的:用高效液相色谱梯度洗脱法同时检测血塞通片中三七皂苷R_1、人参皂苷Rb_1和人参皂苷Rg_1 3种皂苷的含量。方法:用Eclipse XDB—C_8分析柱;乙腈-水二元梯度洗脱;0—15 min(25:75—32:68),平衡5 min;流速1.0 mL·min~(-1);检测波长203 nm。结果:三七皂苷R1、人参皂苷Rg_1和人参皂苷Rb_1的线性范围分别为O.51-3.05,1.68—10.09,2.73—16.39μg。该方法回收率三七皂苷R_1为99.92%(RSD=0.70%)、人参皂苷Rg_1为98.93%(RSD=1.4%)、人参皂苷Rb_1为102.8%(RSD=0.81%)。结论:HPLC梯度洗脱法能将多种皂苷很好地分离检测,提高了时效,减少了误差,结果表明该方法准确可靠,重现性好,结果稳定。     

复方独正片的质量标准研究

目的:建立复方独正片的质量标准。方法:采用薄层色谱法(TLC)对制剂中独正杆、刺老苞、刺五加、三七进行定性鉴别;采用高效液相色谱法测定制剂中紫丁香苷、齐墩果酸、人参皂苷Rg_1、人参皂苷Rb_1、三七皂苷R_1的含量:色谱柱为Inertsil ODS-SP C_(18),流动相为乙腈-水(梯度洗脱),流速为1.0 mL/min,检测波长为215 nm,柱温为25℃,进样量为10μL。结果:独正杆、刺老苞、刺五加、三七的TLC斑点清晰,分离度好,阴性对照无干扰。紫丁香苷、齐墩果酸、人参皂苷Rg_1、人参皂苷Rb_1、三七皂苷R_1检测进样量线性范围分别为0.056~0.337μg(r=0.999 8)、0.022~0.130μg(r=0.999 9)、0.030~0.182μg(r=0.999 5)、0.010~0.061μg(r=0.999 8)、0.038~0.226μg(r=0.999 9);精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为100.55%~103.80%(RSD=2.0%,n=9)、100.00%~104.56%(RSD=3.0%,n=9)、97.06%~102.94%(RSD=2.1%,n=9)、97.06%~102.94%(RSD=2.0%,n=9)、96.67%~100.00%(RSD=1.5%,n=9)。结论:该研究所建标准可用于复方独正片的质量控制。     

胶束电动毛细管色谱法分离分析三七中的人参皂苷Rg1、人参皂苷Re和三七皂苷R1

目的:用胶束电动毛细管色谱法分离测定三七中人参皂苷 Rg_1、人参皂苷 Re 和三七皂苷 R_1 3种皂苷含量。方法:采用Beckman MDQ 电泳仪,40 cm×50 μm的熔融石英毛细管,有效柱长30 cm,缓冲液为20 mmol·L~(-1)SDS、40 mmol·L~(-1)胆酸钠、60 mmol·L~(-1)硼砂,检测波长200 nm。结果:人参皂苷 Rg_1低、中、高剂量的平均加样回收率分别为101.5%,100.6%,100.4%,RSD 分别为2.4%,2.2%,1.0%;人参皂苷 Re 低、中、高剂量的平均加样回收率分别为101.3%,99.23%,99.66%,RSD 分别为2.0%,1.3%,1.1%;三七皂苷 R_1低、中、高剂量的平均加样回收率分别为100.6%,100.5%,100.7%,RSD 分别为1.1%,1.1%,0.86%。结论:本方法能够将三七药材中人参皂苷 Rg_1、人参皂苷 Re 和三七皂苷 R_1完全分离,具有灵敏度高、快速、易于重现且所用试剂价格低廉的特点,因此适合于中药三七的测定,并对今后三七的鉴别和质量控制具有重要意义。     

RP-HPLC法测定固天泉胶囊中人参皂苷Rg1的含量

目的:通过对人参皂苷Rg_1的定性和定量的检测来控制固天泉胶囊的质量。方法:RP-HPLC法。以人参皂苷Rg_1为指标,测定固天泉胶囊中人参皂苷Rg_1的含量。采用Eclipse XDB-C_8柱(4.6mm×150mm,5μm),流动相:乙腈-0.5％磷酸水溶液(20:80),流速:1.0ml·min~(-1),检测波长:205nm,柱温:40℃。平均加样回收率为95.6％,RSD=3.1％(n=5)。结论:用本法测定固天泉胶囊中人参皂苷Rg_1的含量,操作简便,结果准确。     

通脉降脂片质量标准研究

目的 通脉降脂片的质量标准研究.方法 采用薄层色谱法鉴别川芎、三七,用HPLC法测定人参皂苷Rg1的含量.色谱柱:Angilent ZORBAX SB-C18(4.6×150 mm,5μm),流动相为:乙腈-水二元梯度洗脱,检测波长:203nm;流速1.0mLml·min-1;进样量5μL.结果 能准确对川芎、三七进行定性鉴别;人参皂苷Rg1在0.434～3.906μG范围内呈良好的线性关系(r=1.0000);平均回收率为97.62%(n=9,RSD=2.19%).结论 本法快速、简便、准确、重现性好,可作为控制通脉降脂片质量的方法.     

藤丹胶囊质量标准方法的改进

目的完善藤丹胶囊的质量标准。方法修订川芎、黄芪、三七的TLC方法、增加丹参、防己的TLC方法,建立HPLC法测定三七中人参皂苷Rg_1、人参皂苷Rb_1、三七皂苷R1的含量和丹参中丹酚酸B的含量测定。三七的含量测定:以Agilent 5 TC-C_(18)(250mm×4.6mm,5μm)为色谱柱;以乙腈为流动相A,以0.1%磷酸溶液为流动相B进行梯度洗脱;流速1.0m L/min;柱温:35℃;丹参的含量测定:以Agilent Extend C_(18)(250mm×4.6mm,5μm)为色谱柱;流动相:乙腈-1%甲酸溶液(20︰80);流速:1.0m L/min;柱温:35℃。结果三七皂苷R1进样量在1.1545~4.1562μg、人参皂苷Rg_1进样量在5.833~20.9988μg、人参皂苷Rb_1进样量在3.849~13.8564μg、丹酚酸B进样量在1.1~6.6μg范围内,与峰面积呈良好的线性关系,r=0.9998、r=0.9999、r=0.9996、r=0.9999;加样回收率分别为:平均回收率分别为98.39%、101.11%、101.11%,104.05%。结论完善后的质量标准可行,能有效控制藤丹胶囊的质量。     

HPLC法测定含三七类保健食品中三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1含量

目的 建立HPLC法测定保健食品中三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1含量的方法.方法 Waters Symmetry ShieldTM C18(250mm×4.6mm,5μm)色谱柱;柱温:30℃;流动相为乙腈-水,梯度洗脱;检测波长为203nm.结果 三七皂苷R1、人参皂苷Rg1、Re和Rb1分别在6.322~151.716μg·mL-1(r=0.9996)、25.043~601.029μg·mL-1(r=0.9999)、6.292~151.008μg·mL-1(r=0.9991)和25.018~600.430μg·mL-1(r=0.9999)范围内的线性关系良好;平均加样回收率分别为99.53%(RSD=1.18%,n=9),99.70%(RSD=1.34%,n=9),100.38%(RSD=1.15%,n=9)和99.94%(RSD=1.92%,n=9).结论 本法简便、准确、重现性好,可作为含三七类保健食品的质量控制方法.     

UPLC同时测定复方三七胶囊中人参皂苷Rg_1、Re、Rb_1和三七皂苷R_1

目的建立同时测定复方三七胶囊中人参皂苷Rg1、Re、Rb1和三七皂苷R1的UPLC方法。方法采用UPLC,ACQUITY BEH C18色谱柱(2.1mm×100mm,1.7μm),乙腈-水为流动相梯度洗脱,流速为0.45m L/min,检测波长为203nm,柱温为25℃。结果人参皂苷Rg1、Re、Rb1和三七皂苷R1分别在19.61~392.2μg/m L(r=0.9997)、4.813~96.26μg/m L(r=0.9998)、19.92~398.4μg/m L(r=0.9998)和4.850~97.00μg/m L(r=0.9999)线性关系良好,平均加样回收率(n=9)分别为100.00%、99.78%、99.92%和99.83%,RSD分别为0.30%、0.45%、0.29%和0.54%。结论方法快速有效,适用于测定复方三七胶囊中人参皂苷Rg1、Re、Rb1和三七皂苷R1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.

     

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.     

Gender-related symptoms and correlates of alcohol dependence among men and women with a lifetime diagnosis of alcohol use disorders

This study explored gender-related symptoms and correlates of alcohol dependence in a crosssectional study of 150 men and 150 women with a lifetime diagnosis of alcohol use disorders (AUD). Participants were recruited in equal numbers from treatment settings, correctional centres and the general community. Standardized measures were used to determine participants' use of substances, history of psychiatric disorders and psychosocial stress, their sensation seeking and family history of substance use and mental health disorders. Multivariate analyses were used to detect patterns of variables associated with gender and the lifetime severity of AUD. Men had a longer history of severe AUD than women. Women had similar levels of alcohol dependence and medical and psychological sequelae as men, despite 6 fewer years of AUD. More women than men had a history of severe psychosocial stress, severe dependence on other substances and antecedent mental health problems, especially mood and anxiety disorders. There were differences in family history of alcohol-related problems approximating same-gender aggregation. The severity of a lifetime AUD was predicted by its earlier age at onset and the occurrence of other disorders, especially anxiety, among both men and women. The limitations in the generalizability of these findings due to sample idiosyncrasies are discussed.     

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.