HPLC法同时测定阿奇霉素滴眼液中阿奇霉素及苯扎氯铵的含量

目的建立一种高效液相色谱法同时测定阿奇霉素滴眼液中阿奇霉素及苯扎氯铵的含量。方法采用十八烷基硅烷键合硅胶色谱柱(4.6 mm×150 mm,5μm),柱温30℃,以乙腈-磷酸盐缓冲液(取0.05 mol.L-1磷酸氢二钾溶液,用20%磷酸调节pH至8.2)(58∶42)为流动相;检测波长210 nm;流速:1.0 mL.min-1。结果阿奇霉素在1.002 8～5.014 0 mg.mL-1的浓度范围内,苯扎氯铵在6.15μg.mL-1～14.35μg.mL-1的浓度范围内均呈线性。阿奇霉素的平均回收率100.68%,RSD为0.50%(n=9);苯扎氯铵的平均回收率100.59%,RSD为0.92%(n=9)。阿奇霉素与苯扎氯铵的定量限分别为750 ng.mL-1、46 ng.mL-1,平均含量分别为106.94%及100.04%,RSD分别为0.94%及0.67%。仪器重复性RSD值均在2.0%以下。结论本方法简单、准确,可同时测定样品中阿奇霉素及苯扎氯铵的含量。     

双氯芬酸钠滴眼液中苯扎氯铵的测定

目的采用HPLC双氯芬酸钠滴眼液中苯扎氯铵的含量。方法乙腈-5 mmol.L-1醋酸铵溶液（含1%三乙胺,用冰醋酸调节pH值至5.0±0.5）（65∶35）为流动相,CNW色谱柱（150 mm×4.6 mm,5μm）,检测波长为214 nm。结果苯扎氯铵的测定在12.50～125.00μg.mL-1与峰面积线性关系良好,苯扎氯铵的平均回收率为99.0%,RSD为1.3%。结论方法简单、灵敏度高,可用于双氯芬酸钠滴眼液中苯扎氯铵的测定。     

复方门冬维甘滴眼液中苯扎氯铵的测定

目的：建立测定复方门冬维甘滴眼液中苯扎氯铵含量的方法。方法：采用Agilent Zorbax C18色谱柱（150 mm ×4.6 mm,5μm）,以乙腈-5 mmol·L^-1醋酸铵溶液（含1%三乙胺,用冰醋酸调节pH至5.0＆#177;0.5）（65∶35）为流动相,流速为1.0 ml·min^-1,检测波长为214 nm。结果：苯扎氯铵在50.00~150.00μg·ml^-1范围内与峰面积线性关系良好,r=0.9980;平均回收率为99.1%,RSD为0.6%。结论：该方法简便,迅速,灵敏度高,具有良好的重复性及回收率,可用于复方门冬维甘滴眼液中苯扎氯铵的测定。     

盐酸卡替洛尔滴眼液中抑菌剂最适浓度考察及抑菌效力评价

目的 探索盐酸卡替洛尔滴眼液中苯扎氯铵的最适添加浓度。方法 根据苯扎氯铵药敏试验结果,选择抑菌剂浓度范围在5 μg?mL-1～70 μg?mL-1的盐酸卡替洛尔滴眼液进行初步抑菌效力考察,筛选出适宜的抑菌剂添加量。分别于不同苯扎氯铵浓度的盐酸卡替洛尔滴眼液中加入一定浓度的金黄色葡萄球菌、大肠埃希氏菌、铜绿假单胞菌、白色念珠菌菌悬液和黑曲霉孢子悬液,进行挑战实验,测试上述微生物在不同时间点的存活情况。结果 40 μg?mL-1的苯扎氯铵对5种挑战微生物的生长有良好的抑制作用,且为最低有效剂量。结论 40 μg?mL-1的苯扎氯铵可作为盐酸卡替洛尔滴眼液中抑菌剂的最适添加浓度。     

HPLC法测定氧氟沙星滴眼液中抑菌剂的含量

摘要：目的 建立测定氧氟沙星滴眼液中羟苯甲酯、羟苯乙酯、羟苯丙酯、苯扎溴铵或苯扎氯铵的高效液相色谱法。方法 : 采用资生堂 ACR -C18 （250mm×4.6mm,5μm）色谱柱,以1%三乙胺溶液（用磷酸调节pH值至3.0）为流动相A,甲醇为流动相B进行梯度洗脱,检测波长为262nm。结果: 羟苯甲酯、羟苯乙酯、羟苯丙酯线性范围均为1~20μg·mL-1（r=1.0000）,苯扎溴铵或苯扎氯铵n-C12H25取代同系物的线性范围均为10~200μg·mL-1（r=1.0000）;平均加样回收率（n=9）分别为99.5%（RSD=0.5%）;100.3%（RSD=0.4%）; 100.2%（RSD=0.4%）;98.9%（RSD=0.8%）;98.1%（RSD=0.5%）。按拟定方法分别对13个企业34个批次样品进行筛查分析,其中羟苯乙酯使用浓度为0.2~0.3mg·mL-1,苯扎溴铵使用浓度为0.1~0.2mg·mL-1,苯扎氯铵使用浓度为0.1mg·mL-1。结论: 本法测定氧氟沙星滴眼液中羟苯甲酯、羟苯乙酯、羟苯丙酯、苯扎溴铵或苯扎氯铵n-C12H25取代同系物准确、可靠、重现性好,[此句不通顺]可作为氧氟沙星滴眼液中羟苯甲酯、羟苯乙酯、羟苯丙酯、苯扎溴铵或苯扎氯铵n-C12H25取代同系物的定量分析方法。     

不同材质滤膜对于加替沙星滴眼液中抑菌剂的吸附性研究

目的：考察加替沙星滴眼液除菌过滤时不同材质滤膜对于苯扎氯铵的吸附性;建立高效液相色谱法测定加替沙星滴眼液中苯扎氯铵的含量。方法：采用材质为聚醚砜（PES）、聚偏二氟乙烯（PVDF）的滤膜过滤加替沙星滴眼液后,收集滤液,于100,500,1 000,1 500,2 000 mL时取样,测定过滤后苯扎氯铵的含量;以水（用1 mol·L^-1高氯酸调pH至2.2±0.05）-乙腈-异丙醇（58：33：9）为流动相等度洗脱;流速1.0 mL·min^-1;柱温40℃;检测波长214 nm。结果：材质为聚偏二氟乙烯（PVDF）的滤膜对于苯扎氯铵有6.3%的吸附,而材质聚醚砜（PES）对于苯扎氯铵无吸附性;苯扎氯铵在11.1~111 μg·mL^-1（222~2 220 ng）浓度范围内呈良好的线性,线性方程为y=22 162x-15 620（r=0.999 9）,平均回收率为100.58%、RSD=0.60%（n=9）,准确度较好。结论：对于加替沙星滴眼液的生产,采用材质为聚醚砜（PES）的滤膜对其中抑菌剂苯扎氯铵无吸附;建立了HPLC法测定加替沙星滴眼液中苯扎氯铵的方法,操作简便,灵敏度高,重复性好,可快速准确用于加替沙星滴眼液中苯扎氯铵含量分析。     

右旋糖酐70甘油滴眼液中苯扎氯铵含量测定方法研究

目的:建立高效液相色谱法测定右旋糖酐70甘油滴眼液中苯扎氯铵的含量。方法:以氰基硅烷键合硅胶为填充剂;以乙腈-0.03 mol.L-1磷酸二氢钠溶液(用1 mol.L-1氢氧化钠溶液调pH至7.0)(43∶57)为流动相;流速:2.0 mL.min-1;柱温:35℃;检测波长214 nm。苯扎氯铵C12、C14、C16之间的分离度应符合规定。结果:苯扎氯铵在1.28～3.00μg范围内与峰面积线性关系良好(r=0.9999,n=7);平均回收率(n=6)为100.9%,RSD=0.9%。结论:该法操作简便,快速、准确,灵敏度高,重复性好,可用于右旋糖酐70甘油滴眼液中苯扎氯铵含量测定。     

硝酸毛果芸香碱滴眼液中苯扎氯铵含量测定

目的:用高效液相色谱法(HPLC)测定硝酸毛果芸香碱滴眼液中苯扎氯铵的含量。方法:色谱柱为CN(HypersilCN,150mm×4.6mm,5μm);流动相为0.03mol/L磷酸二氢钠溶液(用1mol/L氢氧化钠溶液调节pH至7.0)-乙腈(57:43);流速为2mL/min;检测波长为214nm;柱温为35℃;苯扎氯铵C12、C14、C16之间的分离度应符合规定。结果:苯扎氯铵在40～160μg/mL内线性关系良好,Y=12.2281X+6.8814(r=0.9999,n=6),回收率为99.7%～101.9%,RSD=0.66%。结论:该法操作简便,快速、准确、灵敏度高,重复性好,可用于硝酸毛果芸香碱滴眼液中苯扎氯铵的含量测定。     

依诺沙星滴眼液中防腐剂含量的测定

目的建立依诺沙星滴眼液中常用防腐剂苯扎溴铵、苯扎氯铵和羟苯乙酯的HPLC含量测定方法。方法采用C18柱,苯扎溴铵和苯扎氯铵以0.005mol/L的醋酸铵溶液(每1L中含三乙胺10mL,用冰醋酸调节pH值至5.0±0.5)-乙腈(40∶60)为流动相,检测波长214nm,进样量为50μL;羟苯乙酯以0.005mol/L的醋酸铵溶液(每1L中含三乙胺10mL,用冰醋酸调节pH值至5.0±0.5)-乙腈(50∶50)为流动相,检测波长256nm,进样量20μL。结果苯扎溴铵、苯扎氯铵和羟苯乙酯在各自线性范围内呈良好的线性关系,r分别为0.9998、0.9998、0.9999;平均回收率分别为100.6%、100.0%、100.2%(n=9)。结论该方法简单、准确,适用于依诺沙星滴眼液中三种常用防腐剂苯扎溴铵、苯扎氯铵和羟苯乙酯的含量测定。     

HPLC法测定吡嘧司特钾滴眼液中苯扎溴铵和苯扎氯铵的含量

摘要：目的建立HPLC法测定吡嘧司特钾滴眼液中苯扎溴铵和苯扎氯铵的含量。方法色谱柱：C18（4．6mm×150mm,5μm）;流动相：0．02mol·L^-1庚烷磺酸钠溶液（含0．1％三乙胺,用磷酸调节PH为3．45±0．1）-乙腈（35：65）;检测波长：210nm;柱温：40℃。结果苯扎溴铵在49．86～997．2ng范围内线性关系良好（r=0．9999）,最小检出量为0．15ng,平均回收率为97．4％,RSD为1．0％;苯扎氯铵在9．912-24．78ng范围内呈良好的线性关系（r=0．9999）,最小检出量为0．85ng,平均回收率为99．9％,RSD为1．0％。结论本方法简便、快速、准确、灵敏度高、重复性好,可用于吡嘧司特钾滴眼液中苯扎溴铵和苯扎氯铵的含量测定。     

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.     

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.