高效液相色谱法测定消毒饮优化方胶囊中的异嗪皮啶

目的建立消毒饮优化方胶囊中异嗪皮啶的HPLC测定方法。方法采用phenomenexSynergi4UFusion—RP80A柱（250mm×4．60mm,4μm）,流动相为乙腈-1％磷酸（20：80）,体积流量为1．0mL／min,柱温为40℃,检测波长为342am。结果异嗪皮啶进样量在0．1000～1．0000岭与峰面积呈良好的线性关系（r=0．9999）,平均回收率为95．04％,RSD=1．84％（n=6）。结论该方法操作简便、准确、专属性强、重复性好,可用于消毒饮优化方胶囊中异嗪皮啶的含量测定。     

HPLC法比较野生刺五加中的异嗪皮啶

目的 建立刺五加中异嗪皮啶的定量方法,并对主产区采集的刺五加野生药材的不同部位、不同生长年限及不同生长环境的异嗪皮啶的量进行测定,为分析刺五加野生药材的质量提供参考。方法 刺五加异嗪皮啶的提取采用超声提取法,HPLC法测定,色谱柱为Diamonsil C₁₈（250 mm×4.6 mm,5 mm）,流动相为乙腈-0.1%磷酸（20：80）,检测波长344 nm,体积流量1.0 mL/min。结果 异嗪皮啶进样量在16.8～252.0 ng呈现良好的线性关系（r=0.999 9）,平均回收率为100.4%,RSD值为1.0%（n=6）。刺五加不同部位中,皮的异嗪皮啶含量最高,茎次之,根及根茎含量较低。不同生长年限中,5年生刺五加异嗪皮啶含量最高,3年生含量次之,2年以下含量最低。阳坡生长的异嗪皮啶含量高于阴坡生长的药材。总体分析异嗪皮啶的含量黑龙江高于吉林。结论 本方法可操作性强,简便快速,重复性好,回收率高,稳定可靠,可作为刺五加药材的质控方法。鉴于野生药材生长年限不一,分布不集中,与栽培的药材相比含量波动大,因此,在药品生产过程中,根据对中间体或成品中异嗪皮啶含量的要求,有必要建立刺五加药材异嗪皮啶的含量标准,以保证生产药品的质量。     

清咽片质量控制研究

目的 建立清咽片的质量控制方法。方法 采用薄层色谱法对冰片进行定性鉴别;采用高效液相色谱法对没食子酸进行定量测定。色谱柱为翡纳米公司Kromasil C₁₈柱（250 mm×4.6 mm,5 μm）,以乙腈-含0.1%三乙胺的0.1%磷酸水溶液（1∶99）为流动相,体积流量为1 mL/min,检测波长为273 nm。结果 薄层色谱鉴别斑点清晰,阴性样品无干扰;定量测定中没食子酸进样量在0.007 μg～0.035 μg与峰面积线性关系良好（r＝0.999 9）;平均回收率为98.83%,RSD为1.34%（n＝6）。结论 建立的方法操作简单、准确、专属性和重复性好,可用于该制剂的质量控制。     

HPLC-ELSD测定注射用益气复脉(冻干)中葡甲胺

目的 建立HPLC-ELSD法测定注射用益气复脉（冻干）中葡甲胺的量。方法 色谱柱为Waters Sepherisorb SCX（250 mm×4.6 mm,5 μm）,流动相为0.05 mol/L醋酸铵（醋酸调节pH=3.0）-乙腈（57：43）,体积流量1.0 mL/min,柱温40℃,ELSD漂移管温度60℃,载气气体压力137.90 kPa,增益30。结果 葡甲胺进样量在4.351～29.005 μg呈良好的线性关系,r＝0.999 8,平均回收率（n＝9）为100.3%,RSD为2.27%。结论 本实验建立的方法简便、准确、可靠,可用于测定注射用益气复脉（冻干）的质量控制。     

双波长HPLC法同时测定咳喘胶囊中绿原酸与黄芩苷

目的 建立同时测定咳喘胶囊(I)中绿原酸与黄芩苷的高效液相色谱(HPLC)法。方法 采用双波长HPLC法,以甲醇为流动相A,0.4%磷酸溶液为流动相B,梯度洗脱;检测波长为327 nm(绿原酸)、280 nm(黄芩苷),柱温40 ℃,体积流量1.0 mL/min,进样量,10 μL。结果 绿原酸在6.29～41.96 μg线性良好(r＝0.999 9,n=5),黄芩苷在5.78～38.52 μg线性良好(r＝0.999 9,n=5),平均回收率分别为99.7%和100.0%,RSD分别为0.9%和0.9%。结论 本法操作简便,重复性好,可有效控制咳喘胶囊的质量。     

SPE-HPLC法测定强力枇杷露中盐酸可待因

目的 建立反相高效液相色谱测定强力枇杷露中磷酸可待因的方法。方法 采用Eclipse XDB-C₁₈柱（250 mm×4.6mm,5 μm）,乙腈-0.035 mol/L醋酸钠溶液（冰醋酸调pH＝3.5）（25∶75）为流动相,体积流量为1.0 mL/min,检测波长为240 nm,柱温为40℃。结果 磷酸可待因在2.024~40.24 μg/mL线性良好,回归方程为y＝8.18×105x＋12.2（r＝0.999 2）;平均加样回收率为98.2%,RSD为1.0%（n＝6）。结论 该方法快速准确,灵敏度高,用于强力枇杷露中盐酸可待因含量测定,控制药品质量。     

衍生化法分离（2R，4R）-4-甲基-2-哌啶甲酸乙酯酒石酸盐手性异构体

目的 建立衍生化法分离（2R,4R）-4-甲基-2-哌啶甲酸乙酯酒石酸盐（MPFET）3种手性异构体。方法 以2,3,4,6-四-O-乙酰基-β-D-吡喃葡萄糖异硫氰酸酯（GITC）为柱前衍生化试剂,对MPFET手性异构体进行分离,并对衍生化条件进行优化。采用Venusil AQ C₁₈（250 mm×4.6 mm,5 μm）色谱柱作为固定相进行分离、监测和定量。以0.01 mol/L磷酸二氢钾溶液（用磷酸调pH至3.6）-乙腈（60∶40）为流动相,体积流量1.5 mL/min进行等度洗脱,采用紫外检测器,检测波长266 nm;柱温30℃;进样量20 μL。结果 MPFET与2S,4S-异构体分离度为1.76。2S,4R-异构体的线性范围为1.500～8.999 μg/mL,2R,4S-异构体的线性范围为0.255 2～1.531 0 μg/mL,2S,4S-异构体的线性范围为0.250 1～75.000 0 μg/mL,MPFET的线性范围为0.250 1～600.100 0 μg/mL,回收率均在90%～108%内,RSD均不大于3.0%。结论 柱前衍生化法分离MPFET中3种手性异构体,专属性强、准确度高、灵敏度高、重复性好,可用于MPFET手性异构体的分离和质量控制。     

HPLC-ELSD法测定注射用益气复脉(冻干)中钠元素

目的 建立一种用于测定注射用益气复脉（冻干）中钠元素含量的方法。方法 采用强阳离子交换色谱柱（SCX）,以0.05 mol/L乙酸铵（乙酸调节pH至4.8）-乙腈（50：50）为流动相,体积流量为1.0 mL/min,柱温30℃,撞击器“关闭”模式,漂移管温度为90℃,压缩空气流量为2.5 L/min,检测器的增益值为1。结果 钠元素在60～180 μg/mL范围内线性良好（r＝0.999 3）;准确度试验（n＝9）平均回收率为90.4%,RSD为1.8%;注射用益气复脉（冻干）中钠元素质量分数均值为0.48%（0.33%～0.55%）。结论 所建立的方法简单可靠,可用于测定注射用益气复脉（冻干）中钠元素的含量测定。     

HPLC法测定通乐颗粒中2, 3, 5, 4′-四羟基二苯乙烯-2-O-β-D-葡萄糖苷

目的 建立测定通乐颗粒中2, 3, 5, 4′-四羟基二苯乙烯-2-O-β-D-葡萄糖苷的方法。方法 采用HPLC法,色谱柱为Phenomenex C₁₈柱,检测波长为320 nm,流动相为乙腈-水（20∶80）,体积流量为1.0 mL/min。结果 2, 3, 5, 4′-四羟基二苯乙烯-2-O-β-D-葡萄糖苷在10～100 μg/mL与峰面积呈良好线性关系（r＝0.999 7）,平均回收率为99.74%。结论 本方法准确、简便、重复性好,可用于通乐颗粒中2, 3, 5, 4′-四羟基二苯乙烯-2-O-β-D-葡萄糖苷的含量测定。     

原子吸收分光光度法测定芩连抗病毒合剂中的铅

目的 建立芩连抗病毒合剂中铅含量测定的原子吸收分光光度法。方法 采用石墨炉原子吸收法,检测波长为283.3 nm,灯电流为9 mA,狭缝宽度为0.5 nm。结果 铅的质量浓度在0～0.20 μg/mL与吸光度线性关系良好r＝0.999 5,回收率为98.7%,RSD＝2.1%（n＝3）。结论 所建方法能够简便、快速、准确的测定芩连抗病毒合剂中铅的含量。     

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.

     

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.