RP-HPLC法测定磺苄西林钠的含量及其有关物质

目的:建立RP-HPLC法测定磺苄西林钠的含量及其有关物质.方法:采用C18柱,流动相为0.05 mol·L-1磷酸二氢钾溶液-乙腈(88:12),流速1.0 mL·min-1,检测波长220 nm,柱温30℃.结果:磺苄西林钠的线性范围为0.306 3～0.714 7 g·L-1,r=0.999 9,磺苄西林钠与杂质能完全分离.结论:HPLC法测定结果与微生物检定法比较无显著性差异.本方法可准确、快速、简便地测定磺苄西林钠的含量及其有关物质.     

超高效液相色谱串联质谱法分析磺苄西林钠原料中的杂质

目的建立超高效液相色谱串联质谱法分析磺苄西林钠原料中的杂质,并初步确定杂质的结构。方法采用Acquity UPLC BEH C18色谱柱,以10 mmol.L-1乙酸铵溶液-甲醇(90∶10)为流动相,以电喷雾电离源负离子模式进行质谱数据采集。结果获得磺苄西林和磺苄西林杂质的色谱图以及液相色谱图对应的质谱图,对谱图进行分析归纳,推测磺苄西林样品中2个未知杂质的结构分别为磺苄西林噻唑酸和磺苄西林噻唑酸甲酯化产物。结论本方法快速、灵敏、专属性高,对磺苄西林钠的生产和质量控制具有指导意义。     

超高效液相色谱串联质谱法分析磺苄西林钠原料中的杂质

目的利用超高效液相色谱串联质谱法对磺苄西林钠原料中的杂质分析。方法色谱柱选择Acqiuty UPLC BEH C18,流动相则选择10 mmol/L乙酸铵溶液-甲醇,采集质谱数据则利用电喷雾电离源负离子模式来完成。结果通过分析得到磺苄西林、磺苄西林杂质的色谱图和液相色谱图相对应的质谱图,总结分析谱图,对磺苄西林样品中的未知杂质结构进行推测,分别为磺苄西林噻唑酸和磺苄西林噻唑酸甲酯化产物。结论利用超高效液相色谱串联质谱法对磺苄西林钠原料中的杂质分析,具有较高的专属性和灵敏性,而且快速,对生产磺苄西林钠和控制其质量具有非常重要的作用。     

分子排阻色谱法测定注射用磺苄西林钠中高分子聚合物

目的建立测定注射用磺苄西林钠中高分子聚合物的方法。方法采用Sephadex G 10凝胶色谱柱,以pH7.0的0.1 mol•L－1磷酸盐缓冲液［0.1 mol•L－1磷酸氢二钠溶液：0.1 mol•L－1磷酸二氢钠溶液（61：39）］为流动相A,以水为流动相B,流速1.5 mL•min－1,检测波长254 nm。结果磺苄西林高分子聚合物与磺苄西林能较好分离,磺苄西林对照品在进样量为含磺苄西林0.59～47.46 μg范围内,线性关系良好（r＝0.999 9）;供试品溶液在20.68～40.48 mg•mL－1范围内,溶液浓度与聚合物峰面积呈良好线性关系（r＝0.999 4）;重复性较好（RSD＝4.3%,n＝5）;重现性较好（RSD＝4.8%,n＝3）。结论该方法简便,结果可靠,可以用于注射用磺苄西林钠中高分子聚合物的检测。     

D-(-)-α-磺苄西林钠的合成工艺改进

改进D-(-)-α-磺苄西林钠的合成工艺.方法以苯乙酸为起始原料,经磺化、碱化、离子交换后得消旋的磺苯乙酸,制得磺苯乙酰氯后,与6 - APA缩合得到磺苄西林的非对映异构体.通过重结晶的方法分离出D-(-)-α-磺苄西林,再与异辛酸钠成盐制得目标化合物.结果及结论成功地制备了D-(-)-α-磺苄西林钠,缩短了合成路线并...     

凝胶色谱法测定注射用磺苄西林钠的聚合物

目的建立凝胶色谱法测定注射用磺苄西林钠中聚合物的方法。方法采用高效液相色谱法,色谱柱为Sephadex G-10凝胶柱．流动相A为pH7．0的0．05mol·L^-1磷酸盐缓冲液[0．05mol·L^-1磷酸氢二钠溶液-0．05mol·L^-1磷酸二氢钠溶液（61：39）]、流动相B为水．流速为0．5mL·min^-1,检测波长为254nm。结果磺苄西林在50．72-405．76μg·mL^-1与峰面积呈良好的线性关系（r=0．9999）。结论本方法简便、准确、灵敏度高、重现性好。     

比浊法自动测定注射用磺苄西林钠的效价

目的建立比浊法测定注射用磺苄西林钠效价的方法。方法以金黄色葡萄球菌为试验菌,加菌量为0.5%（V/V）,（37±0.5）℃培养3.5～4.0h测定。结果抗生素最佳线性浓度范围为12.0～25.0U.mL-1,平均回收率为99.9%（n=9）,RSD为1.9%。结论本方法灵敏、快速、实用,可作为测定注射用磺苄西林钠效价的方法。     

HPLC法测定磺苄西林钠中的有关物质

目的建立磺苄西林钠中有关物质的测定方法。方法采用反相高效液相色谱法,以十八烷基硅烷键合硅胶为填充剂,乙腈-四丁基氢氧化铵溶液为流动相;检测波长为220nm,测定磺苄西林钠中有关物质的含量。结果回收率为98.3%,RSD为5.7%,最低定量限为0.41ng。结论本法操作简便,结果准确,可用于磺苄西林钠中有关物质的控制。     

磺苄西林钠在呼吸道系统治疗效果观察

目的探索研究磺苄西林钠治疗呼吸道系统感染的具体效果,为临床应用寻求依据。方法 90例呼吸道系统感染患者随机分为研究组和对照组,各45例。研究组应用磺苄西林钠进行治疗,对照组应用呋苄西林钠进行治疗,将两组研究对象的临床疗效以及细菌清除情况进行对比分析。结果研究组痊愈率为80.00%,显著高于对照组的60.00%;研究组总有效率为97.78%,显著高于对照组的82.22%;研究组细菌清除率为84.21%,显著高于对照组的64.10%,上述组间差异均具有统计学意义(P<0.05)。两组不良反应发生率均为2.22%,差异无统计学意义(P>0.05)。结论应用磺苄西林钠对呼吸道系统感染患者进行治疗,效果好,细菌清除率高,有利于促进患者康复,具有较高的推广应用价值。     

葡聚糖凝胶柱层析法分离测定注射用阿洛西林钠中的聚合物

目的建立一种利用葡聚糖凝胶柱分离测定注射用阿洛西林钠中聚合物的方法。方法注射用阿洛西林钠中的高分子杂质的定量测定是利用葡聚糖凝胶柱色谱法。色谱柱：XK16/40SephadexG-10,柱长：35cm;流动相A为pH7.0,0.025mol·L^-1磷酸盐缓冲液,流动相B为超纯水,流速：1.5mL·min^-1,检测波长254nm,进样量200μL。结果注射用阿洛西林钠在浓度为5.0～60mg·mL^-1的范围内与其峰面积呈良好的线性关系（r为0.9990）。结论本法用于注射用阿洛西林钠中的高分子杂质的测定,灵敏度高,准确性好。     

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.     

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.     

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.     

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.