多波长HPLC法同时测定皮肤康洗液中5种有效成分的含量

摘 要 目的：建立多波长切换高效液相色谱法同时测定皮肤康洗液中芍药苷、甘草苷、甘草酸铵、大黄素和蛇床子素5种有效成分的含量。方法: 色谱柱为 Diamonsil C18柱(200 mm×4.6 mm,5 μm);流动相为乙腈 0.1%盐酸水溶液,梯度洗脱;流速为1.5 ml·min^-1;柱温为30℃;检测波长为232 nm(0～6 min,检测芍药苷)、277 nm(6～10 min,检测甘草苷)、254 nm(10 min以后,检测甘草酸铵、大黄素、蛇床子素）。结果: 芍药苷、甘草苷、甘草酸铵、大黄素和蛇床子素的线性范围分别为28.20～282.0 μg·ml^-1（r=0.999 7）、12.150～121.500 μg·ml^-1（r=0.998 8）、13.420～134.200 μg·ml^-1（r=0.999 5）、0.047～0.466 μg·ml^-1（r=0.999 9）、2.380～23.800 μg·ml^-1（r=0.999 9）,平均加样回收率分别为98.49%,99.00%,98.38%,97.36%,97.70%,RSD分别为0.71%,0.62%,0.85%,0.92%,0.78%（n=6）。结论:该方法简便、准确、灵敏度高、重复性好,可用于同时测定皮肤康洗液中上述5个有效成分的含量。     

HPLC法测定黄连上清片中4种成分的含量

摘 要 目的： 提高黄连上清片质量标准,建立同时测定绿原酸、栀子苷、黄芩苷、盐酸小檗碱4种成分含量的方法。方法: 采用高效液相色谱法,色谱柱为DiamonsilTM C₁₈(250 mm×4.6 mm,5 μm),流动相为二元梯度系统,其中溶剂A为乙腈,溶剂B为0.3%磷酸水溶液,流速为1.0 ml·min^-1,检测波长为238 nm,柱温30℃,进样量为10 μl。结果: 绿原酸、栀子苷、黄芩苷、盐酸小檗碱的线性范围分别为8.11～81.10 μg·ml^-1(r=0.999 7)、13.08～130.80 μg·ml^-1(r=0.999 7)、10.76～107.60 μg·ml^-1(r=0.999 8)、7.92～79.20 μg·ml^-1(r=0.999 8)范围内呈良好的线性关系,平均加样回收率分别为99.19%(RSD=0.9%)、98.44%(RSD=1.1%)、99.12%(RSD=1.0%)、99.18%(RSD=1.1%)(n=9)。结论:该方法简便、准确、重复性好,可用于黄连上清片的质量控制。     

HPLC波长切换法同时测定九味双解口服液中5种成分的含量

摘 要 目的：建立HPLC波长切换法同时测定九味双解口服液中绿原酸、咖啡酸、木犀草苷、黄芩苷和大黄素的含量。方法: 采用Shiseido Capcell Pak C₁₈（200 mm×4.6 mm,5 μm）色谱柱,流动相为甲醇（A）-0.1%磷酸溶液（B）（梯度洗脱）,流速为1.0 ml·min^-1,柱温为25℃,检测波长(0~19 min,在327 nm波长下检测绿原酸;19~25 min,在323 nm波长下检测咖啡酸;25~35 min,在350 nm波长下检测木犀草苷;35~55 min,在320 nm波长下检测黄芩苷;55~60 min,在254 nm波长下检测大黄素)。结果: 绿原酸、 咖啡酸、木犀草苷、黄芩苷和大黄素的线性范围分别为0.34～6.8 μg·ml^-1（r=0.999 9）、0.23～4.56 μg·ml^-1（r=0.999 5）、1.32～26.38μg·ml^-1（r=0.999 9）、9.60～192.01μg·ml^-1（r=0.999 9）、1.14～22.80μg·ml^-1（r=0.999 6）;平均加样回收率分别为99.50%（RSD=0.52%）、99.10%（RSD=1.43%）、98.83%（RSD=0.94%）、99.98%（RSD=0.21%）、99.22%（RSD=0.82%）（n=9）。结论:本文建立的含量测定方法,具有操作简便、结果准确、重现性良好的特点,可用于九味双解口服液的质量控制。     

HPLC法同时测定玉真散中天麻素、升麻素苷、5-O-甲基维斯阿米醇苷、欧前胡素、异欧前胡素的含量

摘 要 目的：建立HPLC法同时测定玉真散中天麻素、升麻素苷、5-O-甲基维斯阿米醇苷、欧前胡素、异欧前胡素含量。方法: 色谱柱为Phenomenex Gemini C18柱（250 mm×4.6 mm,5 μm）,柱温为25℃,流速为1.0 ml·min^-1 ,流动相为甲醇 水梯度洗脱,检测波长为230 nm,进样量为5 μl。结果: 天麻素在2.68~214.00μg·ml^-1范围内线性关系良好（r=0.999 9）,平均回收率为100.2％,RSD为0.9％（n=6）;升麻素苷在5.22~418.00 μg·ml^-1范围内线性关系良好（r=0.999 7）,平均回收率为99.9％,RSD为0.9％（n=6）;5-O-甲基维斯阿米醇苷在4.57~365.80 μg·ml^-1范围内线性关系良好（r=0.999 5）,平均回收率为99.7％,RSD为1.0％（n=6）;欧前胡素在5.22~417.20μg·ml^-1范围内线性关系良好（r=0.999 6）,平均回收率为99.0％,RSD为0.9％（n=6）;异欧前胡素在5.29~423.20μg·ml^-1范围内线性关系良好（r=0.999 8）,平均回收率为100.2％,RSD为0.8％（n=6）。结论: 该方法简单、准确,可同时测定5种成分的含量,可用于玉真散的质量控制。     

HPLC法测定枳实消痞丸中芸香柚皮苷、柠檬苦素、和厚朴酚及厚朴酚含量

摘 要 目的： 建立高效液相色谱法同时测定枳实消痞丸中芸香柚皮苷、柠檬苦素、和厚朴酚及厚朴酚含量的分析方法。方法: 色谱柱为岛津Shim-pack VP-ODS C18柱（250 mm×4.6 mm,5 μm）,流动相A为乙腈 甲醇(1∶2),流动相B为水,梯度洗脱,流速为1.0 ml·min^-1,柱温为30℃,进样量为20 μl;芸香柚皮苷检测波长为λ1=283 nm,柠檬苦素检测波长为λ2=210 nm,和厚朴酚、厚朴酚检测波长为λ3=294 nm。结果: 芸香柚皮苷、柠檬苦素、和厚朴酚、厚朴酚分别在5.26～105.20μg·ml^-1（r=0.999 8）、7.65～153.00 μg·ml^-1（r=0.999 4）、6.21～124.20 μg·ml^-1（r=0.999 3）、6.45～129.00 μg·ml^-1（r=0.999 6）范围内线性关系良好,平均加样回收率(n=6)分别为99.00％（RSD=0.77％）、98.17％（RSD=1.19％）、98.78％（RSD=0.86％）、97.90％（RSD=0.99%）。结论:该方法简便、准确、可靠,可用于枳实消痞丸的质量控制。     

HPLC法同时测定蒲药灌肠液中3个有效成分的含量

摘 要 目的： 建立蒲药灌肠液中香蒲新苷、异鼠李素-3-O-新橙皮苷和延胡索乙素的HPLC含量测定方法。方法: 采用ZORBAX SB-C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以乙腈-0.1%磷酸（三乙胺调节pH至6.0）为流动相,梯度洗脱程序,流速:1.0 ml·min^-1,检测波长为254 nm（0～14 min）和281 nm（14～25 min）,柱温:30 ℃。结果: 香蒲新苷、异鼠李素-3-O-新橙皮苷和延胡索乙素的线性范围分别为19.840～198.400 μg·ml^-1（r=0.999 6）、20.520～205.200 μg·ml^-1（r=0.999 8）和10.040～100.400 μg·ml^-1（r=0.999 7）,回收率分别为98.8%、98.6%和98.9%,RSD分别为1.4%、1.6%和1.3%（n=6）。结论: 该方法灵敏度高,专属性强,可用于蒲药灌肠液的质量控制。     

HPLC法同时测定小儿咳喘灵颗粒中6种成分

摘 要 目的：建立利用HPLC法采取波长变换同时测定小儿咳喘灵颗粒中盐酸麻黄碱、（R,S） 告依春、苦杏仁苷、绿原酸、甘草苷、甘草酸含量的方法。方法: 色谱条件：Agilent Eclipse XDB C18（250 mm×4.6 mm,5 μm）,以乙腈 0.1%磷酸为流动相,梯度洗脱,流速为1.0 ml·min^-1 ,测定波长为207 nm（盐酸麻黄碱、苦杏仁苷）、237 nm（甘草酸、甘草苷、绿原酸）、245 nm[（R,S） 告依春）]。结果:盐酸麻黄碱进样浓度在2.423～96.920 μg·m^-1 范围与峰面积线性关系良好,r=0.999 2,平均回收率为100.1%(RSD=0.30%,n=6);（R,S） 告依春进样浓度在1.920～76.798 μg·m^-1 范围与峰面积线性关系良好,r=0.999 9,平均回收率为99.86%(RSD=1.14%,n=6);绿原酸进样浓度在2.396～92.891 μg·m^-1 范围与峰面积线性关系良好,r=0.999 9,平均回收率为98.57%(RSD=0.75%,n=6);苦杏仁苷进样浓度在1.982～79.279 μg·m^-1 范围与峰面积线性关系良好, r=0.999 8,平均回收率为99.67%(RSD=0.59%,n=6);甘草苷进样浓度在2.136～85.440 μg·m^-1 范围与峰面积线性关系良好, r=0.999 9,平均回收率为98.57%(RSD=0.69%,n=6);甘草酸进样浓度在2.432～97.260 μg·m^-1 范围与峰面积线性关系良好,r=0.999 9,平均回收率为98.57%(RSD=0.11%,n=6)。结论:该方法准确、重复性好,可用于小儿咳喘灵颗粒的质量控制。     

HPLC波长切换法测定氨咖黄敏胶囊4个成分的含量

摘 要 目的： 建立HPLC波长切换法同时测定氨咖黄敏胶囊中4个成分的含量。方法: 采用Agilent ZORBAX SB C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以乙腈（A）-甲醇（B）-磷酸二氢铵溶液（取0.1 mol·L^-1磷酸二氢铵溶液1 000 ml ,加磷酸1 ml,混匀）（C）为流动相,梯度洗脱,流速1.0 ml·min^-1,柱温 35℃,变换波长时间为（0～9 min ：225 nm;9～38 min ：450 nm）。结果: 采用HPLC波长切换法测定氨咖黄敏胶囊4个成分的含量,线性范围分别为：对乙酰氨基酚24.680～394.900 μg·ml^-1（r=0.999 9）,马来酸氯苯那敏0.201～3.214 μg·ml^-1（r=0.999 9）,咖啡因1.129～18.070 μg·ml^-1（r=0.999 9）,胆红素0.010～0.165 μg·ml^-1（r=0.999 8）;平均回收率分别为：99.25% (RSD=0.46%), 99.29% (RSD=0.32%),99.49% (RSD=0.48%)及99.75% (RSD=0.55%)（n=6）。结论:该法简单,灵敏,准确,重复性好,可用于氨咖黄敏胶囊的含量测定。     

HPLC法同时测定大败毒胶囊中绿原酸、咖啡酸和阿魏酸的含量

摘 要 目的: 建立HPLC法同时检测大败毒胶囊中绿原酸、咖啡酸和阿魏酸的测定方法。方法: 采用Agilent C₁₈（250 mm×4.6 mm,5 μm）色谱柱;乙腈-0.4%磷酸溶液（15∶85）为流动相,流速：1.0 ml·min^-1;检测波长：324 nm。柱温:30℃,进样量：10 μl。结果:线性范围：绿原酸5.42～32.43 μg·ml^-1(r=0.999 8),咖啡酸2.63～26.32 μg·ml^-1(r=0.999 4),阿魏酸1.44～14.44 μg·ml^-1(r=0.999 9);平均回收率：绿原酸99.98%,RSD=0.2%(n=6),咖啡酸99.31%,RSD=0.4%(n=6),阿魏酸99.48%,RSD=0.8%(n=6)。结论:该方法操作简便、准确,重复性好,可用于测定大败毒胶囊中绿原酸、咖啡酸和阿魏酸的含量。     

ASE-HPLC法快速测定决明子中大黄酚和橙黄决明素

摘 要 目的：建立快速溶剂萃取（ASE）及HPLC测定决明子中大黄酚和橙黄决明素的分析方法。方法: 利用正交试验对ASE350快速溶剂萃取系统进行提取方法的研究,采用HPLC法同时测定决明子中大黄酚和橙黄决明素的含量。色谱柱为ACE Excel C18 PFP柱(75 mm×2.1 mm,2.5 μm),流动相为乙腈 0.1%磷酸溶液梯度洗脱,流速为0.4 ml·min^-1,检测波长为284 nm,柱温为40℃。结果: 采用甲醇为萃取溶剂、萃取温度为120℃、静态萃取时间为5 min以及循环萃取3次的方法最优,可以很好地提取决明子中大黄酚和橙黄决明素,耗时仅为药典提取方法的1/9。大黄酚和橙黄决明素线性范围为0.73~58.57 μg·ml^-1(r=0.999 7)和1.09~87.29 μg·ml^-1（r=0.999 6),平均回收率分别为102.7%（RSD=0.8%）和98.2%（RSD=1.5%）。 结论:该方法能简便、快速、准确的测定决明子中的大黄酚和橙黄决明素。     

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.     

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.