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。     

GC-MS法定性定量分析贴敷类医疗器械中樟脑、薄荷脑、冰片

摘 要 目的:利用气相色谱-质谱联用仪（GC-MS）建立贴敷类医疗器械中樟脑、薄荷脑、冰片的定性和定量分析方法。方法: 采用Agilent HP-INNOWax (30 m×0.25 mm,0.25 μm)毛细管色谱柱;以氦气为载气,流量为1.0 ml·min^-1;柱温80℃维持2 min,以10℃·min^-1的升温速率升至120℃,维持12 min,再以30℃·min^-1的升温速率升至200℃,维持3 min;离子源为电子轰击电离（EI）源,采集模式为全扫描/选择离子检测。结果:能检测出样品中是否添加樟脑、薄荷脑、冰片,并对其进行定量。3种化合物的线性范围分别为1.742～2.177×10³(r=0.998 9),1.982～2.478×10³(r=0.998 9),1.999～2.499×10³ μg·ml^-1(r=0.999 8),线性关系均良好;平均回收率分别为93.3%,98.8%,94.9%(n=9)。结论:方法简便、灵敏、准确、快速,可用于贴敷类医疗器械中樟脑、薄荷脑、冰片的定性和定量检测。     

黄芪饮片中4个异黄酮类成分的含量测定

摘 要 目的:建立高效液相色谱法测定黄芪饮片中4个异黄酮成分的含量方法。方法: 色谱柱为Agilent Zorbax SB-C₁₈(250 mm×4.6 mm,5 μm) ,流动相为乙腈-水梯度洗脱,流速1.0 ml·min^-1,检测波长为260 nm, 柱温30℃,进样量10 μl。结果:毛蕊异黄酮-7-葡萄糖苷、芒柄花苷、毛蕊异黄酮、芒柄花素分别在4.42～442 μg·ml^-1、2.06～206 μg·ml^-1、3.36～336 μg·ml^-1、4.60～460 μg·ml^-1浓度范围内与各自峰面积积分值呈良好的线性关系;平均回收率分别为99.4%(RSD=5.34%)、94.8%(RSD=2.39%)、98.9%(RSD=3.69%)、102.3%(RSD=3.01%)(n=9)。结论:本方法简便、准确、重复性好,可用于黄芪饮片的质量控制。     

GC-MS法测定甲磺酸达比加群酯中的致突变杂质

目的 建立一种气相色谱-质谱联用法（GC-MS）同时测定甲磺酸达比加群酯中甲磺酸甲酯、甲磺酸乙酯和甲磺酸异丙酯的方法。方法 采用DB-624色谱柱（30 m×0.25 mm,1.4 μm）;程序升温：起始温度100 ℃,以15 ℃·min^-1的速率升温至200 ℃,再以25 ℃·min^-1的速率升温至240 ℃;进样口温度为220 ℃,载气为氦气,流速为1.0 mL·min^-1,进样量为2.0 μL。采集模式为选择离子监测（SIM）,离子源温度为230 ℃。通过内标法进行计算。结果 三种甲磺酸酯之间的分离度均大于2.0,甲磺酸甲酯、甲磺酸乙酯、甲磺酸异丙酯的线性回归方程分别为Y=0.0130X+0.0524（r=0.999 0）、Y=0.0249X+0.0633（r=0.999 3）、Y=0.0188X+0.0906（r=0.998 5）,均在5.0～120.0 ng·mL^-1浓度范围内线性关系良好。检出限为1.5 ng·mL^-1（0.15 ppm）,定量限为5 ng·mL^-1（0.5 ppm）。甲磺酸甲酯、甲磺酸乙酯和甲磺酸异丙酯的平均回收率分别为96.28%、97.91%和95.87%,RSD分别为2.83%、2.93%和1.73%。结论 本方法简便、快速、准确、专属性强、灵敏度高,适用于甲磺酸达比加群酯中三种甲磺酸酯的检测。     

离子色谱法测定炎琥宁原料药中碳酸盐

目的 建立离子色谱法测定炎琥宁原料药中碳酸盐残留的方法。方法 采用离子色谱法。色谱柱：Dionex IonPac AS18（250 mm×4 mm）;淋洗液：0.022 mol/L氢氧化钾;体积流量：1.0 mL/min;进样体积：10 μL;柱温：30 ℃;检测器：电导检测器;检测池温度：35 ℃;抑制器：Dionex ASRS 300（4 mm）。结果 CO₃^2-与Cl^-、NO₂^-、NO₃^-、SO₄^2-分离良好,CO₃^2-在10～120 μg/mL与峰面积呈良好的线性关系（r=0.999 0）;平均回收率为102.1%,RSD值为3.7%（n=9）。结论 该方法灵敏、准确、简便,专属性好,可用于测定炎琥宁原料药中碳酸盐的残留。     

HPLC法测定乙酰谷酰胺中异构体的含量

目的 建立高效液相色谱法测定乙酰谷酰胺中异构体N-乙酰-D-谷氨酰胺的含量测定方法。方法 采用高效液相色谱法,直链淀粉-三（S）-α-甲苯基氨基甲酸酯为填充剂（AS-H 4.6 mm×250 mm,5 μm）手性色谱柱;检测波长210 nm,柱温30 ℃,流动相为正己烷（每1 000 mL加0.5 mL三氟乙酸和0.5 mL三乙胺）：无水乙醇（每1 000 mL中加0.5 mL三氟乙酸和0.5 mL三乙胺）=90:10。结果 浓度在1.289 3~36.099 5 μg·ml^-1范围内线性关系良好（r=0.998 2,n=5）,平均回收率94.9%,RSD=1.6%（n=9）,方法的检测限LOD为0.314 6 μg·ml^-1,定量限1.258 4 μg·mL^-1。结论 所用方法专属性强、结果准确、稳定性好,适用于乙酰谷酰胺中异构体N-乙酰-D-谷氨酰胺的检测。     

HPLC法测定黄连上清片中连翘酯苷A的含量

目的 采用高效液相色谱法测定黄连上清片中连翘酯苷A的含量。方法 色谱柱：VP-ODSC₁₈色谱柱（4.6 mm×250 mm,5 μm）,流动相：乙腈-0.4%冰醋酸溶液（15:85）,流速1.0 mL·min^-1,检测波长330 nm。结果 连翘酯苷A在10.24 ~81.92 µg·mL^-1范围内与峰面积线性关系良好(r=0.999 8),精密度试验RSD为0.85%,重复性试验RSD为1.14%,平均回收率为97.91%,RSD为1.55%(n=6)。结论 该方法操作简单,精密度良好,结果准确可靠,适用于黄连上清片中连翘酯苷A的含量测定。     

高效液相色谱法测定苍辛滴鼻剂中绿原酸及木兰脂素的含量

目的 运用高效液相色谱法对苍耳子中的绿原酸及辛夷中的木兰脂素进行含量测定。方法 绿原酸采用高效液相色谱法,色谱柱为Shim-Pack CLC ODS C18柱（250×4.6 mm,5 μm）;乙腈-0.4%磷酸溶液（10∶90）为流动相;检测波长为327 nm;流速：1.0 mL/min。木兰脂素的色谱条件为：用辛基键合硅胶为填充剂Hypersil C8柱（250×4.6 mm,5 μm）为色谱柱;乙腈-四氢呋喃-水（35∶1∶64）为流动相;检测波长为278 nm;流速：1.0 mL/min。结果 绿原酸在12.99～129.90 μg/mL（r=0.999 9）范围内及木兰脂素在19.67～196.70 μg/mL（r=0.999 9）范围内线性关系良好,绿原酸回收率为99.28%,RSD为1.15%（n=9）;木兰脂素回收率为99.42%,RSD为0.68%（n=9）, 3批样品中绿原酸的平均含量为0.818 4、0.818 5、0.818 9 mg/mL;木兰脂素的平均含量为0.163 7、0.163 4、0.164 1 mg/mL。结论 高效液相色谱法简便、灵敏、准确,可作为苍辛滴鼻剂的定量质量控制。     

HPLC法测定肝素钠注射液中6种抑菌剂

目的 建立高效液相色谱（HPLC）法同时测定肝素钠注射液中苯酚、苯甲醇、三氯叔丁醇、羟苯甲酯、羟苯乙酯、羟苯丙酯6种抑菌剂。方法 采用Agilent Zorbax SB-C₁₈（4.6 mm×250 mm,5 μm）色谱柱,流动相A为水,流动相B为甲醇,梯度洗脱,流速为1.0 mL·min^-1,检测波长为220 nm及256 nm,柱温30 ℃。结果 苯酚、苯甲醇、羟苯甲酯、羟苯乙酯、三氯叔丁醇、羟苯丙酯分别在25.00~400.06 μg·mL^-1（r=1.000 0）、104.49~1 671.88 μg·mL^-1（r=0.999 9）、30.65~490.4 μg·mL^-1（r=0.999 9）、5.36~85.81 μg·mL^-1（r=0.999 9）、49.60~793.54 μg·mL^-1（r=0.999 9）、5.03~80.45 μg·mL^-1（r=1.000 0）内线性关系良好,平均回收率分别为100.3%、99.7%、99.8%、100.0%、99.4%和100.1%,RSD分别为1.0%、1.2%、1.3%、1.4%、1.4%和1.4%（n=9）。结论 方法准确,重现性好,结果可靠,可用于肝素钠注射液中6种抑菌剂的测定。     

HPLC法测定安立生坦中R异构体

目的 建立HPLC法测定安立生坦中R异构体的方法。方法 采用HPLC法, 用硅胶键合蛋白质型手性色谱柱ULTRON ES-OVM(150 mm×4.6 mm, 5 μm);以0.02 mol/L磷酸二氢钾溶液(用磷酸调节pH至4.0)-乙腈(80:20)为流动相;检测波长220 nm;柱温30 ℃;体积流量为1.0 mL/min;进样体积20 μL。结果 安立生坦R异构体在0.501～4.008 μg/mL与峰面积线性关系良好(r=0.999 3), 平均回收率为98.62%, RSD值为2.82%(n=12)。结论 本法操作简便快速, 结果准确可靠, 可用于安立生坦中R异构体的控制。     

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.

     

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.