HPLC法同时测定跌打丸中3种有效成分的含量

目的 探讨建立同时测定跌打丸中芍药苷、川续断皂苷Ⅵ和丹皮酚含量的方法。方法 采用Agilent ZORBAX C₁₈色谱柱（4.6 mm×250 mm,5 μm）;流速为0.8 mL·min^-1,以乙腈（A）-0.1%磷酸水溶液（B）为流动相,进行梯度洗脱;检测波长为230,212,274 nm。结果 芍药苷进样量在0.514 8~1.544 5 μg与峰面积线性关系良好（r=0.999 7）,平均回收率为97.01%（RSD=0.94%,n=6）。川续断皂苷Ⅵ在3.023 8~9.071 4 μg线性关系良好（r=0.999 2）,平均回收率为98.44%（RSD=0.26%,n=6）。丹皮酚在0.101 2~0.303 6 μg线性关系良好（r=0.999 8）,平均回收率为97.84%（RSD=0.42%,n=6）。结论 建立的方法简便可行,重复性好,灵敏度高,可有效控制跌打丸的质量。     

HPLC法测定复方苯海拉明乳膏中盐酸苯海拉明的含量

目的 建立HPLC法测定复方苯海拉明乳膏中盐酸苯海拉明的含量。方法 色谱柱为ACE5C₁₈S/N-A66766柱（150 mm×4.6 mm,5 μm）;流动相为甲醇-水-三乙胺（70:30:0.67,用磷酸调pH为6.5）;检测波长设定230 nm;流速设定1.0 ml/min;乳膏经过提取净化后进样20 μl在室温下分析。结果 盐酸苯海拉明在39.52～197.6 μg/ml范围内线性关系良好（r=0.999 7）,平均回收率为100.5%（RSD=1.25%,n=9）,重复性结果显示RSD为0.78%（n=6）,所测得盐酸苯海拉明乳膏含量结果为标示量的101.3%、99.83%、99.62%。结论 本方法准确、灵敏、专属性强、重现性好,对复方苯海拉明乳膏质量控制标准的提高具有参考意义。     

CO2超临界流体色谱法同时测定莪术油中3个倍半萜类成分的含量

目的 建立CO₂超临界流体色谱法测定莪术油中呋喃二烯、牻牛儿酮和莪术二酮含量的方法。方法 采用ACQUITY UPC² HSS C₁₈ SB色谱柱（3.0 mm×150 mm,1.8 μm）,以CO₂-乙腈为流动相,梯度洗脱;流速为1.0 mL·min^-1;检测波长为216 nm,柱温为55℃,背压为2 000 psi。结果 呋喃二烯在2.67~1 337.26μg·mL^-1内线性关系良好（r=1.000）,加样回收率为97.94%（n=6,RSD=1.50%）。牻牛儿酮在2.77~1 386.00 μg·mL^-1内线性关系良好（r=1.000）,加样回收率为96.07%（n=6,RSD=1.68%）;莪术二酮在6.99~3 493.00 μg·mL^-1内线性关系良好（r=1.000）,加样回收率为99.33%（n=6,RSD=1.88%）。结论 本方法快捷准确、稳定且绿色环保,可用于莪术油中上述3个倍半萜类成分的质量控制。     

HPLC测定肾炎宁片中大黄酸、大黄素、大黄酚及雷公藤甲素的含量

目的 建立HPLC测定肾炎宁片中大黄酸、大黄素、大黄酚及雷公藤甲素的含量。方法 大黄酸、大黄素、大黄酚的测定采用流动相为甲醇-0.1%磷酸（70∶30）,检测波长为254 nm;雷公藤甲素采用流动相为乙腈-水（25∶75）,检测波长为220 nm;两者均采用Lichrospher-C₁₈柱（4.6 mm×250 mm,5 mm）,流速均为1.0 ml·min^-1。结果 大黄酸、大黄素、大黄酚以及雷公藤甲素分别在1.83~14.64 μg·ml^-1（r=0.999 9）,2.895~23.16 μg·ml^-1（r=0.999 8）,7.625~61.00 μg·ml^-1 （r=0.999 8）以及1.52~24.32 μg·ml^-1（r=0.999 6）内与峰面积呈良好的线性关系,大黄酸平均回收率为103.2%,RSD=1.73% （n=9）;大黄素平均回收率为98.6%,RSD=3.94%（n=9）;大黄酚平均回收率为98.3%,RSD=2.54%（n=9）;雷公藤甲素平均回收率为99.61%,RSD=2.83%（n=9）。结论 本方法准确、可靠、专属性强,可作为该制剂的定量控制方法。     

HPLC双波长法测定复方罗布麻片Ⅰ中泛酸钙和氢氯噻嗪的含量

目的 建立HPLC双波长法测定复方罗布麻片Ⅰ中泛酸钙和氢氯噻嗪的含量。方法 采用Kromasil C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以含0.1%辛烷磺酸钠溶液（用磷酸调节pH值至3.0）-乙腈（96：4）为流动相A,以甲醇为流动相B,采用梯度洗脱,柱温为35℃,检测波长泛酸钙200 nm、氢氯噻嗪275 nm,流速为1.0 mL·min^-1,进样量为10 μL。结果 泛酸钙和氢氯噻嗪分别在0.025~0.5 μg（r=0.999 6）和0.16~3.2 μg（r=1.000 0）内线性关系良好;平均加样回收率（n=9）分别为101.2%（RSD=0.47%）和101.6%（RSD=0.49%）。结论 本法精密度好,结果准确可靠,适用于该制剂的质量检验分析。     

HPLC法测定妥布霉素滴眼液中5种抑菌剂

目的 建立同时测定妥布霉素滴眼液中5种抑菌剂(羟苯乙酯、硫柳汞、羟苯丙酯、苯扎溴铵和苯扎氯铵)的HPLC方法。方法 采用Agilent Zorbax SB-C₁₈ (4.6 mm×150 mm,5 μm)色谱柱,流动相A为1%三乙胺（磷酸调节pH值至3.5±0.05）;流动相B为甲醇,梯度洗脱,流速为1.0 mL·min^-1,柱温35 ℃,检测波长为214 nm。结果 羟苯乙酯、硫柳汞、羟苯丙酯、苯扎溴铵/苯扎氯铵各峰均分离良好;羟苯乙酯在0.77～192.5 μg·mL-1范围内线性关系良好(r=0.999 5),平均回收率为100.0%(RSD=0.9%,n=9);硫柳汞在2.16～541.0 μg·mL^-1范围内线性关系良好(r=0.999 7),平均回收率为100.1%(RSD=0.6%,n=9);羟苯丙酯在0.84～209.8 μg·mL^-1范围内线性关系良好(r=1.000 0),平均回收率为100.3%(RSD=1.0%,n=9);苯扎溴铵在4.36～1090 μg·mL^-1范围内线性关系良好(r=0.9992),平均回收率为100.2%(RSD=0.5%,n=9);苯扎氯铵（n-C12H25）3.22～805.0 μg·mL^-1范围内线性关系良好(r=0.999 8),平均回收率为100.1%(RSD=1.1%,n=9);苯扎氯铵（n-C14H29）1.66～413.9 μg·mL^-1范围内线性关系良好(r=1.000 0),平均回收率为100.1%(RSD=0.6%,n=9)。结论 该方法准确、灵敏、简便,可用于妥布霉素滴眼液中羟苯乙酯、硫柳汞、羟丙丙酯、苯扎溴铵及苯扎氯铵5种抑菌剂的检查。     

百贝益肺胶囊含量测定的方法改进

目的 增加评价指标,建立科学、合理的百贝益肺胶囊含量测定方法。方法 C₁₈小柱纯化样品,优化色谱条件为：Vp-ODS色谱柱（150 mm×4.6 mm,5 μm）;柱温：20℃;变动流速;流动相：乙腈（A）-水（B）,梯度洗脱;进样量：10 μL;检测波长：203 nm。结果 所测成分三七皂苷R₁、人参皂苷Rg₁、人参皂苷Rb₁分别在40.24~241.44（r=0.999 6）,91.50~549.00（r=0.999 9）,35.72~241.32（r=0.999 8）μg·mL^-1内线性关系良好;加样回收率为94.15%~99.81%,RSD为1.12%~1.94%。结论 该方法准确,重复性良好,可为修订标准提供依据。     

HPLC-UV-ELSD法同时测定青蒿中青蒿素、青蒿乙素和青蒿酸的含量

用HPLC-UV-ELSD法同时测定青蒿药材中青蒿素、青蒿乙素和青蒿酸的含量。采用Nucleodur C₁₈色谱柱(250 mm×4.6 mm，5 μm ID)；以乙腈-0.1%乙酸水(50∶50)为流动相；紫外检测波长209 nm,蒸发光散射检测器漂移管温度50 ℃。结果显示，青蒿素、青蒿乙素和青蒿酸能够达到很好分离。它们的线性范围分别为0.52～2.6 μg， r=0.999 4(n=5)； 0.022～4.4 μg， r=0.999 9(n=5)； 0.203～8.12 μg，r=0.999 8(n=5)。平均回收率分别为99.45%(RSD=2.3%， n=6)；102.37%(RSD=1.7%， n=6)；101.10%(RSD=0.79%， n=6)。本法简单、准确、快速，可同时测定青蒿药材中青蒿素、青蒿乙素和青蒿酸的含量。     

HPLC法测定麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量

目的 建立麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量测定方法。方法 采用高效液相色谱（HPLC）法,色谱柱：Wondasil C₁₈（4.6 mm×250 mm,5 μm）;流动相：乙腈-0.1%磷酸溶液（5：95）;流速：1 ml/min;检测波长：215 nm;柱温：30℃;进样量：10 μl。结果 盐酸麻黄碱、盐酸伪麻黄碱的质量浓度分别在4.231~42.31 μg/ml（r=0.999 7）、1.187~11.87 μg/ml（r=0.999 9）范围内与各自峰面积线性关系良好,平均加样回收率为分别为98.9%、98.1%;RSD分别为0.48%、0.64%。结论 该法准确度高、重复性好, 可用于麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量测定。     

用HPLC法同时测定自制复方特比萘酚软膏中3个主药成分的含量

目的 建立同时测定自制复方特比萘酚软膏中3个主药成分含量的HPLC法。方法 色谱柱为ZORBAX SB-C₈柱（4.6 mm×250 mm,5 μm）,流动相为甲醇-0.1%磷酸溶液（70∶30）,柱温：30 ℃,流速：1.0 ml/min,检测波长：248 nm,进样量：10 μl。结果 盐酸特比萘芬在20.4～204.0 μg/ml（r =0.999 7）,莫匹罗星在40.4～404.0 μg/ml（r=0.9998）,糠酸莫米松在2.02～20.20 μg/ml（r=0.999 7）的浓度范围呈良好的线性关系,加样回收率分别为99.39%、99.21%、99.97%,RSD分别为0.82%、0.59%、0.81%（n=9）。结论 该方法的专属性、重复性良好,可用于自制复方特比萘酚软膏中的特比萘酚、莫匹罗星、糠酸莫米松的含量测定。     

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.