毛细管色谱法测定洛美沙星中的有机溶剂残留量

目的：建立毛细管气相色谱法测定洛美沙星中的有机溶剂残留量。方法：用INNOWAX毛细管气相色谱柱，FID检测器，以2-戊酮为内标进行测定。结果：乙酸乙酯、四氢呋喃、乙醇、乙腈的线性范围分别为0～80μg／ml(r=0．9997)、0～11．52μg／ml(r=0．9996)、0～80μg／ml(r=0．9997)，0～6．56μg／ml(r=0．9996)；平均回收率分别为100．5％、100．1％、101．2％、100．1％；RSD分别为1．30％、0．9％、1．18％和1．23％(n=9)。结论：本方法简单、准确、灵敏度高、重现性好，适用于洛美沙星中有机溶剂残留量的测定。     

柱前衍生化-高效液相色谱法测定白念珠菌中多胺的含量

目的建立同时测定白念珠菌中4种多胺（腐胺、尸胺、亚精胺和精胺）的HPLC方法。方法样品经苯甲酰氯衍生化,资生堂C18色谱柱（100mm×3．0mm,3．0μm）分离,以甲醇（A）-0．1％甲酸水（B）为流动相进行梯度洗脱,0～5min,30％-48％B;5—12min,48％B;12～15min,48％～70％B;15～25min,70％b,流速0．6ml／min,检测波长254nm。结果腐胺、尸胺、亚精胺和精胺浓度分别在0．775—77．50μg／ml（r=0．9999）、1．160～116．0μg／ml（r=0、9999）、5．800～580．0μg／ml（r=0．9998）、2．533～192．7μg/ml（r=0．9999）的范围内线性关系良好。4种多胺的加样回收率为94．27％～109．3％,精密度RSD〈4％。结论该含量测定方法灵敏、重现性好,能同时测定白念珠菌中4种多胺的含量。     

复方气喘合剂中四种组分的毛细管区带电泳安培检测法测定

采用毛细管区带电泳-安培检测法测定了气喘合剂中氨茶碱、那可汀、盐酸甲氧那明和盐酸麻黄碱的含量，Cu修饰的碳纤维电极对四组分均显示出高催化活性，且稳定性好。四组分的线性范围分别为1.3～28μg/ml（r=0．997）、0．6～17μg／ml（r=0．992）、0．4～13μg／ml（r=0．996）、0．5～10．3μg／ml（r=0．995）。平均回收率分别为99．3％（RSD2．1％）、99．3％（RSD2．3％）、101．4％（RSD1．9％）、98．7％（RSD3．1％）。     

HPIC法测定天麻素氯化钠注射液中天麻素的含量

目的：建立HPLC测定天麻素氯化钠注射液中天麻素的含量。方法：用HypersilBDS（5um，4．6mm＊250mm）C18柱；以甲醇-0．01mol／L磷酸二氢钠（8：92，磷酸调节PH至4．0±0．1）为流动相；流速0．8ml／min；检测波长220hm；进样量2μl。结果：天麻素在2．5μg／ml～25μg／ml范围内，天麻素浓度与峰面积的线性关系良好（r=0．9998），检测限为1．15ng（S／N=3）。回收率为98．9％，R5D=0．08％（n=9）。结论：方法简便，结果准确，重复性好。     

HPLC法同时测定感冒喷雾剂主药含量

目的：建立同时测定感冒喷雾剂中盐酸萘甲唑林和马来酸氯苯那敏含量的HPLC法。方法：采用ODS柱，以乙腈-1．0％十二烷基硫酸钠-冰醋酸(65:35:0．3)为流动相，检测波长为264nm。结果：盐酸萘甲唑林Y=19132．4X 11486．8，r=0．9999(n=5)，线性范围15．18～25．31μg／ml，回收率99．6％,RSD0．60％(n=5)。马来酸氯苯那敏Y=14214．3X 45201．5，r=0．9999(n=5)，线性范围76．56～127．6μg／ml，回收率99．8％。RSD0．63％(n=5)。结论：本法方便、快捷、准确、精密度高，适用于感冒喷雾剂的含量测定。     

HPLC法同时测定紫草凡士林中5种萘醌类化合物的含量

目的：建立同时测定紫草凡士林中紫草素、乙酰紫草素、乙酰氧基异戊酰紫草素、异丁酰紫草素和β,β’-二甲基丙烯酰紫草素含量的方法。方法：采用高效液相色谱法。色谱柱为AgilentEclipseXDB．C18（250mm×4．6mm,5um）,流动相为甲醇．乙腈-0．2％甲酸溶液（48：32：20,V／V／V）,流速为1．0ml／min,柱温为24℃,检测波长为516nln。结果：紫草素、乙酰紫草素、乙酰氧基异戊酰紫草素、异丁酰紫草素和β,β’-二甲基丙烯酰紫草素的质量浓度分别在7．12～71．20μg／ml（r=O．9994）、11．92～119．20μg／ml（r=0．9996）、4．07~40．70μg／ml（r=0．9997）、3．65～36．50μg／ml（r=0．9996）、5．11～51．10ug／m1（r=0．9995）范围内与各自峰面积积分值呈良好的线性关系;平均加样回收率分别为100．82％、101．49％、97．99％、100．29％、101．74％,RSD分别为3．03％、1．25％、1．75％、2．25％、2．31％（”均为6）。结论：该方法简单易行、结果准确、重复性好,适用于紫草凡士林的质量控制。     

HPLC法测定益母丸中盐酸水苏碱的含量

目的：建立高效液相色谱法测定益母丸中盐酸水苏碱的含量测定方法。方法：采用醋酸乙酯、乙醇-强酸性阳离子交换树脂纯化去杂方法制备供试品溶液,以ODS-3柱为色谱柱;甲醇-0．05mol／L磷酸二氢钾溶液(65：28)为流动相;流速为1ml／min;检测波长为215nm;按外标法进行检测。结果：盐酸水苏碱进样量在1．16～14．50tμg良好的线性关系,r=0．9997;样品平均加样回收率为98．19／5(n=5),RSD为1．46％;重复性实验RSD为1．18％(n=5)。结论：方法简便、准确重现性好,可作为益母丸的含量测定方法。     

酚氨咖敏颗粒含量测定方法的改进

目的：建立HPLC法同时测定酚氨咖敏颗粒中对乙酰氨基酚、咖啡因、氨基比林的含量。方法：色谱柱：Kromasil C18（250mm×4．6mm,5μm）;流动相：1％醋酸溶液（用三乙胺调pH为3．5）-甲醇-乙腈（65：10：25）;流速：1．0ml·min^-1;检测波长：273nm;柱温：30℃。结果：对乙酰氨基酚的线性范围为12．3～123．2μg·ml^-1（r=0．9996）,平均回收率为98．65％,R．如为0．31％（n=5）;咖啡因的线性范围为2．44～24．42μg·ml^-1（r=0．9998）,平均回收率为99．15％,RSD为0．15％（n：5）;氨基比林的线性范围为8．23～82．34μg·ml^-1（r=0．9999）,平均回收率为98．40％,RSD为0．39％（n=5）。结论：方法简单可行,可用于酚氨咖敏颗粒中对乙酰氨基酚、咖啡因、氨基比林的含量测定。     

HPLC法测定云南白药中三七皂苷R1、人参皂苷Rg1及人参皂苷Rb1含量

目的：建立高效液相色谱法同时测定云南白药中三七皂苷R。、人参皂苷Rg。Rb。含量方法。方法：采用ShimadzuVP—ODSC。8色谱柱（150mm×4．6mm,5μm）,流动相：乙腈．水梯度洗脱;流速为1．0ml·min-1;检测波长为203nm。结果：三七皂苷R1、人参皂苷Rg1及Rb1的线性范围分别为0．12～0．81μg,r=0．9999,1．31—9．17μg,r=0,9999及0．13～0．91μg,r=0．9998,回收率分别为：98．9％（RSD=2．55％）,98．7％（RSD=1．26％）及99．3％（RSD=1．60％）。结论：方法简便、准确、舌舅性妤．可用干该相l剂古白席詈控制．     

复方厄贝沙坦片中厄贝沙坦和氢氯噻嗪的HPLC测定

建立同时测定复方厄贝沙坦片中厄贝沙坦和氢氯噻嗪含量的HPLC方法。用Inertsil ODS-3色谱柱，流动相为乙腈-0．08mol／L磷酸溶液(用三乙胺调至pH5．0)(40：60)，检测波长225nm。厄贝沙坦和氢氯噻嗪分别在15～135μg／ml(r=0．9999)和1．2～10．8μg／ml(r=0．9999)浓度范围内线性关系良好，方法平均回收率分别为100．0％(RSD=0．46％)和100．5％(RSD=0．49％)。     

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.