RAM—HPLC测定人血清及房水中丝裂霉素的浓度

目的:建立一种快捷、灵敏的高效液相色谱法测定肿瘤病人血清及青光眼患者手术后房水中丝裂霉素(MMC)浓度的方法。方法:使用 Waters HPLC 仪,配有限进介质填料(RAM)直接进样固定相,甲醇-水为10:90,流速为0.8 mL·min~(-1)的流动相,紫外二极管阵列检测器,测定了胃癌、胆囊癌及肝癌病人化疗后的血清及青光眼患者手术后房水中 MMC 的浓度。结果:MMC 与血清及房水中的蛋白质有良好的分离,保留时间为5.6 min。在40～200μg·L~(-1)水中及50～2000μg·L~(-1)血清中浓度范围内均显良好的线性关系,r 分别为0.9912与0.9991,日内变异<4%,日间变异<8%,回收率近100%。结论:RAM-HPLC 法,样品不经前处理,简单快速,精密度好,用此法可用于包含 MMC 的化疗方案的监测及药动学的研究。     

高效液相色谱法测定兔房水中氟脲嘧啶和丝裂霉素的含量

目的:测定壳聚糖膜和免眼房水中氟脲嘧啶(5-Fu)和丝裂霉素(MMC)的含量.方法:使用Waters HPLC仪,配有浸透限制固定相(RAM)直接进样,流动相为甲醇-水(10:90),流速为0.8 mL·imin-1,紫外二极管阵列检测器,测定溶液和房水中的5 Fu、MMC浓度.结果:5-Fu和MMC与房水中的蛋白质有良好的分离,保留时间分别为3.8 min和5.6 min.两种药物在规定的浓度范围内都显良好的线性关系,日内RSD＜4%,日间RSD＜7%,平均回收率分别为99.50%和99.04%.结论:RAM-HPLC法样品不经前处理,简单快速,精密度好,回收率高.当壳聚糖膜吸附了5-Fu和MMC置于兔眼内时,用本法已测定了其释放药物过程.     

RAM-HPLC法测定肝癌病人血浆中丝裂霉素浓度

目的建立一种快捷、灵敏的高效液相色谱法测定肝转移癌病人血浆中丝裂霉素(MMC)浓度的方法。方法用HPLC仪,配有限进介质(RAM)直接进样固定相及紫外二极管阵列检测器,测定肝转移癌病人动脉灌注丝裂霉素后血药浓度,用3P97软件进行模拟,计算其药代动力学参数。结果MMC在50～2000ug·L-1内线性关系良好,日内变异<4%,日间变异<8%,回收率近100%。在肝癌病人中,Cmax为1.19μg·mL-1,AUC为60.51μg·min·mL-1。结论本方法样品不经前处理,简单快速,精密度好,可用于肝动脉灌注MMC化疗方案的药代动力学研究。     

不同方法提取的香椿子挥发油的气质联用成分分析

目的:采用超临界 CO_2流体萃取法及水蒸气蒸馏法从香椿籽中提取挥发油,用气相色谱-质谱联用技术对其化学成分进行分析。方法:采用超临界 CO_2流体萃取法与水蒸气蒸馏法从香椿籽中提取挥发油,用归一化法测定其百分含量。用气相色谱-质谱法对化学成分进行鉴定。色谱条件:DB-5毛细管柱(30 m×0.25 mm,0.25μm);程序升温:初始温度60℃,保持5 min,以4℃·min~(-1)升至180℃,保持10 min,再以15℃·min~(-1)升至260℃,保持50 min;分流进样,分流比50:1;进样口温度280℃。结果:超临界 CO_2流体萃取法提取的挥发油共鉴定了63种成分,占挥发油总成分的88%以上;水蒸气蒸馏法提取挥发油共鉴定了50种成分,占挥发油总成分的94%以上。结论:超临界 CO_2流体萃取法提取的挥发油能更真实、全面地反映药材中的化学成分。     

AVL 9130电解质分析仪测定氯化钠注射液含量

目的:用AVL9130电解质分析仪测定氯化钠注射液中氯化钠含量。方法:利用氯化钠注射液中的Na~ 浓度与人体血清中的离子浓度相近,样品不需任何处理,直接测定。结果:平均回收率为100.1％(RSD=0.01％);样品测定结果与银量法比较基本一致。结论:本法操作简单、快速,结果准确,可用于该制剂的含量测定。     

高效液相色谱-蒸发光散射检测法测定芪黄胶囊中黄芪甲苷的含量

目的:研究芪黄胶囊中黄芪甲苷含量测定的前处理方法,并建立以高效液相色谱-蒸发光散射检测(HPLC-ELSD)法测定芪黄胶囊中黄芪甲苷含量的方法。方法:采用溶剂提取结合中性氧化铝进行样品前处理,用HPLC法,以蒸发光散射检测器测定黄芪甲苷含量。色谱柱为Kromasil C18,流动相为乙腈-水(30∶70),流速为0.8ml/min;ELSD参数气体流速为2.0ml/min,漂移管温度为90℃;进样量为10μl。结果:黄芪甲苷进样量在0.8μg~8μg范围内呈现良好的线性关系(r=0.9 998);平均回收率为99.2%(RSD=1.2%)。结论:本试验中前处理方法能有效除去芪黄胶囊复方中杂质对黄芪甲苷的干扰,所建立的含量测定方法操作简便、快速、准确、适用范围广。     

GC法测定复方苦参注射液中聚山梨酯80的含量

目的:建立测定复方苦参注射液中聚山梨酯80含量的气相色谱方法。方法:采用脂肪酸甲酯化法进行样品前处理。气相色谱条件:DB-WAX毛细管柱(PEG-20000,30 m×0.32 m×0.25 m);氢火焰离子化检测器(FID);进样口温度250℃,检测器温度为250℃;柱温初始温度为80℃,以10℃.min-1升温至220℃,保持20 min;载气为氮气,恒定流速1 mL.min-1,进样方式为分流进样,分流比10∶1;进样量为1μL。结果:聚山梨酯80的进样浓度在0.1～5.0 mg.mL-1(r=0.9998)范围内呈良好线性关系;平均回收率(n=3)为97.4%～100.7%。结论:该方法简便快速,可用于复方苦参注射液中聚山梨酯80的含量测定。     

维生素C片含量测定方法的改进

中国药典1995年版规定维生素Ｃ片(ＶＣ片)用碘量法测定含量。测定过程中对样品进行前处理很麻烦。为此,我们对ＶＣ片在进行前处理和未进行前处理2种情形下,按中国药典规定的碘量法对其进行了比较测定。结果见表1。表1　ＶＣ片含量测定结果比较(标示量%)批号药典法直接滴定法960101962965960420980983960633980985961154968977970209941943970210948951　　从表1可以看出,样品进行或不进行前处理所得结果基本一致。以此提供药典修改时参考维生素C片含量测定方法的改进$陕西省西安制药厂四分厂!710077@吕美丽…     

改进HPLC测定血浆中西沙必利样品的处理方法

目的　改进提取血样中药物的方法 ,以提高测定灵敏度。方法　将血浆样品用 2 . 0mol·L-1NaOH碱化 ,先用混合溶媒正己烷 -乙醚 -异丙醇 (4∶1∶0 . 2 5 )提取样品中的西沙必利 ,然后向含有药物的混合溶媒中加入环己烷 ,再用 0 .5mol·L-1磷酸反提有机溶媒中的药物 ,用磷酸液直接进样。结果　加入环己烷后再用磷酸反提药物 ,可以使回收率至少提高 32 %。结论　这种样品处理方法既消除了杂质对药物测定的干扰 ,也保证了较高的提取回收率。     

人血白蛋白中辛酸钠的含量测定

目的:建立人血白蛋白中辛酸钠含量测定的一个简单快捷方法.方法:采用萃取法测定人血白蛋白中辛酸钠的含量,利用辛酸钠为有机弱酸强碱盐的化学性质及在两种溶剂中分配系数的不同,用乙醚萃取分离出辛酸,然后用标准0.01 mol·L-1氢氧化钠溶液进行酸碱滴定,测其含量,并对其线性关系、精密度、稳定性和回收率进行研究,且与气相色谱法进行比较.结果:人血白蛋白中辛酸钠的含量测定,经典萃取法与气相色谱法无显著性差异(P＞0.05).结论:该方法简单快捷,结果可靠,可用于人血白蛋白中辛酸钠的含量控制.     

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.

     

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.