复方阿奇霉素葡萄糖注射液中阿奇霉素的HPLC测定

建立了HPLC法测定复方阿奇霉素葡萄糖注射液中阿奇霉素的含量.采用ODS柱,流动相为2mmol/L磷酸氢二铵溶液(pH 9.4)-异丙醇-乙腈(15:25:60),流速1ml/min,检测波长210nm.阿奇霉素的线性范围为10～50μg/ml,平均回收率为99.7%(RSD 0.28%).     

高效液相色谱法测定阿奇霉素片中阿奇霉素含量

目的:建立阿奇霉素片含量测定的HPLC法。方法:采用Thermo C18(250 mm×4.6 mm,5μm)色谱柱,流动相为磷酸盐缓冲液(取0.05 mol/L磷酸氢二钾溶液,用20%的磷酸溶液调节pH至8.2)-乙腈(45∶55)为流动相,检测波长为210 nm。结果:阿奇霉素在0～1.4 mg/ml范围内线性关系良好,平均回收率99.6%,RSD为0.56。结论:本方法准确可靠,灵敏度高,重现性好,可用于阿奇霉素片含量测定。     

HPLC法测定注射用门冬氨酸阿奇霉素的含量和有关物质

目的建立注射用门冬氨酸阿奇霉素中阿奇霉素的含量和有关物质测定的HPLC法。方法使用DiamonsilC18柱(250mm×4.6mm,10μm),流动相为0.1mol/L磷酸氢二钾(pH9.0)∶乙腈(55∶45),流速1.2ml/min,检测波长210nm,柱温35℃。结果阿奇霉素在浓度0.5~2.5mg/ml内与峰面积呈良好的线性关系,r=0.9997,平均回收率99.52%,RSD为0.65%(n=9)。结论该方法简便、准确、专属,可用于注射用门冬氨酸阿奇霉素的含量及有关物质的测定。     

阿奇霉素有关物质测定方法的优化

目的 对阿奇霉素有关物质测定方法进行优化.方法 采用SHISEIDO CAPCELL PAK C18 MG Ⅱ(51μm,4.6mm×250mm)色谱柱;磷酸盐缓冲液(0.05mol/L磷酸氢二钾溶液,用20%的磷酸调节pH值至8.2):乙腈(45:55)为流动相;柱温30℃;流速1.0mL/min;检测波长210nm.结果 阿奇霉素在10～1000μg/mL范围内浓度与峰面积呈良好线性关系,r=0.9999;最低检测限为100ng,与其已知杂质分离度良好.结论 本方法可用于测定阿奇霉素及制剂的有关物质.     

高效液相色谱法测定阿奇霉素胶囊含量

目的建立高效液相色谱法测定阿奇霉素胶囊含量。方法色谱柱为Hypersil ODS2(4.6×250 mm);流动相为0.067 mol.L-1磷酸二氢钾溶液(用磷酸调pH为3.5)-乙腈(70∶30);流速为1.0 ml.min-1;柱温:50℃;检测波长:210 nm。结果阿奇霉素在进样量2.5~50μg的范围内与峰面积呈良好线性关系(r=0.9999),平均回收率为100.38%,RSD为0.91%。结论本法简便快捷,结果准确,重现性好,可用于阿奇霉素胶囊的含量测定。     

HPLC法测定阿奇霉素分散片的含量

目的用高效液相色谱法测定阿奇霉素分散片的含量。方法以Hibar RT Pre-Packed柱为固定相,0.1mol.L-10.002M磷酸氢二铵溶液-异丙醇-乙腈(15∶25∶60,pH 9.2)为流动相,流速:1.0ml.min-1,紫外检测波长:210nm的条件下分离测定阿奇霉素分散片。结果阿奇霉素分散片在0.6~3mg.ml-1范围内,浓度与峰面积线性关系良好,r=0.9992,平均回收率为101.2%,RSD为0.8%。结论本法简便、迅速、灵敏度高、重现性好,可用于测定阿奇霉素分散片的含量。     

HPLC法测定阿奇霉素胶囊的含量

目的建立阿奇霉素胶囊含量的HPLC法。方法采用Shim-pack VP-ODS(4.6 mm×150 mm,5 nm)(岛津柱),流动相为0.067 mol.L-1磷酸二氢铵溶液(三乙胺调pH至6.5)-乙腈(74∶26),检测波长200 nm,流速1 ml.min-1,柱温30℃。结果阿奇霉素在0.76~3.82 g.L-1范围内线性关系良好,r=0.999 9,方法的回收率为100.2%(n=3)。结论本法简便、准确、重现性好,结果可靠,可用于阿奇霉素的含量测定。     

梯度洗脱HPLC法测定盐酸平阳霉素及注射药物中的有关物质

目的 建立梯度洗脱HPLC法测定盐酸平阳霉素及注射用盐酸平阳霉素中的有关物质.方法 采用C18(150mm×4.6mm,5μm)色谱柱,己烷磺酸钠溶液(己烷磺酸钠7.53g与乙二胺四乙酸二钠3.72g以0.08mol/L乙酸溶液溶解并稀释至1000ml,用氨溶液调节pH为4.3)为流动相A,甲醇:乙腈(70:30)为流动相B,梯度洗脱,流速1.0ml/min,检测波长254nm,柱温30℃.结果 盐酸平阳霉素溶液在10～500μg/ml范围内,溶液浓度与峰面积呈良好线性关系,r=0.9999;最低检测浓度1μg/ml.结论 本法可用于测定盐酸平阳霉素及注射用盐酸平阳霉素中的有关物质.     

阿奇霉素与胆木注射液联合应用对肺炎双球菌作用的研究

目的 研究阿奇霉素与胆木注射液联合用药对肺炎双球菌解热效果.方法将体重在24 g～30 g的健康小白鼠40只,随机分为4组,每组10只.A组注射胆木注射液,B组注射阿奇霉素,C组注射胆木注射液和阿奇霉素.用量:胆木注射液0.17 ml/10 g,阿奇霉素0.1 ml/10 g,0.9%氯化钠溶液0.1 ml/10 g,肺炎双球菌0.5 ml/只.结果 空白组生理盐水无明显解热作用;注射阿奇霉素、注射胆木注射液都具有明显地解热效果;注射阿奇霉素与胆木注射液有显著增强作用(P＜0.05).结论 阿奇霉素与胆木注射液联用对肺炎双球菌解热效果具有显著增强作用.     

HPLC法测定注射用阿奇霉素磷酸二氢钠的含量及有关物质

目的建立一种高效液相色谱方法来测定注射用阿奇霉素磷酸二氢钠含量及有关物质。方法以Shiseido C18(4.6 mm×250 mm,5μm)色谱柱为分析柱,以磷酸盐缓冲液(0.05 mol·L-1磷酸氢二钾溶液,用20%磷酸溶液调节pH值至8.2)-乙腈(40∶60)为流动相,柱温30℃,检测波长为210 nm,流速为1.0 mL·mim-1。结果阿奇霉素在10⁵ 000μg·mL-1范围内浓度与峰面积呈良好线性关系,r=1.000 0,平均回收率为100.6%,RSD为0.99%(n=9)。结论本方法可快速、准确的测定注射用阿奇霉素磷酸二氢钠含量及有关物质的测定。     

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.     

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.     

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.     

Aquatic Insects and Trace Metals: Bioavailability,Bioaccumulation, and Toxicity

Abstract

The uptake of metals from food and water sources by insects is thought to be additive. For a given metal, the proportions taken up from water and food will depend both on the bioavailable concentration of the metal associated with each source and the mechanism and rate by which the metal enters the insect. Attempts to correlate insect trace metal concentrations with the trophic level of insects should be made with a knowledge of the feeding relationships of the individual taxa concerned. Pathways for the uptake of essential metals, such as copper and zinc, exist at the cellular level, and other nonessential metals, such as cadmium, also appear to enter via these routes. Within cells, trace metals can be bound to proteins or stored in granules. The internal distribution of metals among body tissues is very heterogeneous, and distribution patterns tend to be both metal and taxon specific. Trace metals associated with insects can be both bound on the surface of their chitinous exoskeleton and incorporated into body tissues. The quantities of trace meals accumulated by an individual reflect the net balance between the rate of metal influx from both dissolved and particulate sources and the rate of metal efflux from the organism. The toxicity of metals has been demonstrated at all levels of biological organization: cell, tissue, individual, population, and community. Much of the literature pertaining to the toxic effects of metals on aquatic insects is based on laboratory observations and, as such, it is difficult to extrapolate the data to insects in nature. The few experimental studies in nature suggest that trace metal contaminants can affect both the distribution and the abundance of aquatic insects. Insects have a largely unexploited potential as biomonitors of metal contamination in nature. A better understanding of the physico-chemical and biological mechanisms mediating trace metal bioavailability and exchange will facilitate the development of general predictive models relating trace metal concentrations in insects to those in their environment. Such models will facilitate the use of insects as contaminant biomonitors.