壳聚糖磺胺嘧啶银胶浆；磺胺嘧啶银；高效液相色谱法；含量测定

摘 要 目的: 建立测定壳聚糖磺胺嘧啶银胶浆中磺胺嘧啶银含量的方法。方法: 采用反相高效液相色谱法,以Agilent Eclipse XDB C₁₈为色谱柱（250 mm×4.6 mm,5 μm）,流动相：乙腈 1%磷酸（8∶〖KG-*2〗92）,流速：1 ml·min^-1,检测波长：254 nm,柱温：25℃,进样量：20 μl。结果:磺胺嘧啶银在10～400 μg·ml^-1范围内与峰面积呈良好的线性关系（r=0.999 9）。加样回收率为102.18％,RSD=2.41％。结论:该方法简便、准确、可靠,可用于测定壳聚糖磺胺嘧啶银胶浆中磺胺嘧啶银的含量。     

HPLC法测定复方苯海拉明乳膏中盐酸苯海拉明的含量

目的 建立HPLC法测定复方苯海拉明乳膏中盐酸苯海拉明的含量。方法 色谱柱为ACE5C₁₈S/N-A66766柱（150 mm×4.6 mm,5 μm）;流动相为甲醇-水-三乙胺（70:30:0.67,用磷酸调pH为6.5）;检测波长设定230 nm;流速设定1.0 ml/min;乳膏经过提取净化后进样20 μl在室温下分析。结果 盐酸苯海拉明在39.52～197.6 μg/ml范围内线性关系良好（r=0.999 7）,平均回收率为100.5%（RSD=1.25%,n=9）,重复性结果显示RSD为0.78%（n=6）,所测得盐酸苯海拉明乳膏含量结果为标示量的101.3%、99.83%、99.62%。结论 本方法准确、灵敏、专属性强、重现性好,对复方苯海拉明乳膏质量控制标准的提高具有参考意义。     

氯新酮乳膏质量标准的研究

目的 建立氯新酮乳膏的质量控制方法。方法 采用TLC法对氯新酮乳膏中的新霉素、酮康唑和哈西奈德进行定性鉴别;采用HPLC法对氯新酮乳膏中的酮康唑和哈西奈德进行含量测定;色谱条件为：ZORBAX SB-C₁₈（4.6 mm×150 mm,5 μm）色谱柱;以甲醇-磷酸盐缓冲液（pH=7.40）75∶25为流动相,检测波长235 nm,流速1.0 ml/min;采用旋光法对氯新酮乳膏中的硫酸新霉素进行含量测定。结果 鉴别和含量测定方法均有较好的专属性。酮康唑在1.999~39.98 μg 的范围内呈良好的线性关系（r=0.999 9）,平均回收率为97.75%,RSD为0.77%;哈西奈德在0.400 8~8.016 μg范围内呈良好的线性关系,平均回收率为97.57%,RSD为0.84%。硫酸新霉素的含量测定中,线性范围为130.4~2 608单位/ml,r=0.999 6（n=6）,平均回收率为98.8%,RSD为2.6%。结论 该法可用于氯新酮乳膏的质量控制。     

用HPLC法同时测定自制复方特比萘酚软膏中3个主药成分的含量

目的 建立同时测定自制复方特比萘酚软膏中3个主药成分含量的HPLC法。方法 色谱柱为ZORBAX SB-C₈柱（4.6 mm×250 mm,5 μm）,流动相为甲醇-0.1%磷酸溶液（70∶30）,柱温：30 ℃,流速：1.0 ml/min,检测波长：248 nm,进样量：10 μl。结果 盐酸特比萘芬在20.4～204.0 μg/ml（r =0.999 7）,莫匹罗星在40.4～404.0 μg/ml（r=0.9998）,糠酸莫米松在2.02～20.20 μg/ml（r=0.999 7）的浓度范围呈良好的线性关系,加样回收率分别为99.39%、99.21%、99.97%,RSD分别为0.82%、0.59%、0.81%（n=9）。结论 该方法的专属性、重复性良好,可用于自制复方特比萘酚软膏中的特比萘酚、莫匹罗星、糠酸莫米松的含量测定。     

白蔹药材中大黄素含量的反相高效液相色谱法测定

目的 建立白蔹药材中大黄素含量的测定方法,为完善白蔹药材的质量控制标准提供方法和依据。方法 采用反相高效液相色谱法,色谱柱：Apollo-C₁₈柱（4.6 mm×250 mm,5 μm）;流动相：甲醇-0.2%磷酸（85:15）;流速：1.0 ml/min;柱温：室温;检测波长：220 nm。结果 在选定的色谱条件下,白蔹药材中大黄素在0.124～3.968 μg/ml范围内线性关系良好,直线回归方程为Y=53 962X–966.46,r=0.999 7,平均回收率为99.7%,RSD为2.5%（n=9）。结论 该方法所测结果准确、灵敏度高、重现性好,适用于白蔹药材中大黄素的含量测定。     

HPLC法测定麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量

目的 建立麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量测定方法。方法 采用高效液相色谱（HPLC）法,色谱柱：Wondasil C₁₈（4.6 mm×250 mm,5 μm）;流动相：乙腈-0.1%磷酸溶液（5：95）;流速：1 ml/min;检测波长：215 nm;柱温：30℃;进样量：10 μl。结果 盐酸麻黄碱、盐酸伪麻黄碱的质量浓度分别在4.231~42.31 μg/ml（r=0.999 7）、1.187~11.87 μg/ml（r=0.999 9）范围内与各自峰面积线性关系良好,平均加样回收率为分别为98.9%、98.1%;RSD分别为0.48%、0.64%。结论 该法准确度高、重复性好, 可用于麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量测定。     

HPLC法测定盐酸多沙普仑葡萄糖注射液的含量

目的 建立盐酸多沙普仑葡萄糖注射液的高效液相色谱含量测定方法。方法 采用COSMOSIL C₁₈(150 mm×4.6 mm,5 μm)色谱柱,以0.82 μg/L醋酸钠溶液(用冰醋酸调pH值为4.5) -乙腈=70:30为流动相,检测波长为214 nm。结果 盐酸多沙普仑浓度在13~91 μg/ml范围内呈良好的线性关系(r=0.999 8)。平均加样回收率为99.3%,RSD为0.81%(n=9)。结论 此方法简便、准确、灵敏度高、专属性强。     

UPLC-MS/MS法测定人血浆中丙硫氧嘧啶的含量

目的 建立UPLC-MS/MS法测定人血浆中丙硫氧嘧啶的含量,为临床治疗药物监测（TDM）和生物等效性试验（BE）提供方法学基础。方法 采用Agilent SB-C₁₈柱（4.6 mm×150 mm,5 μm）,流动相为甲醇-0.1%甲酸水溶液（80∶20,V/V）,等度洗脱。质谱采用AJS-ESI源,多反应监测（MRM）正离子模式,检测离子对为：丙硫氧嘧啶m/z 171.1→112.1、内标（丙硫氧嘧啶-D5）m/z 176.1→117.0。结果 血浆中丙硫氧嘧啶在10~5 000 ng/ml范围内线性关系良好,r=0.999 3;批内和批间的精密度和准确度良好（RSD<10%,RE<±10%）;不同浓度的基质效应均<110%,变异系数<5%;不同浓度的平均回收率为101.60%~113.56%,符合方法学要求。结论 该方法快速简便、灵敏准确,适用于血浆中丙硫氧嘧啶的含量测定。     

用HPLC法测定红茴香注射液中槲皮苷的含量

目的 建立高效液相色谱法测定红茴香注射液中槲皮苷的含量。方法 色谱柱为Dikma C₁₈(250 mm×4.6 mm,5 μm),以乙腈-0.1%磷酸水溶液（25∶75）为流动相,流速为1.0 ml/min,柱温30 ℃,检测波长为256 nm。结果 槲皮苷在0.215～3.225 μg范围内呈良好线性关系,相关系数为0.999 6,该法的平均回收率为99.39%,RSD为0.82%（n=6）,重复性为1.194 mg/ml,RSD为0.40%。结论 3批红茴香注射液的槲皮苷平均含量结果为1.191 mg/ml,该法简便、快速、准确, 可作为测定红茴香注射液中槲皮苷含量的方法。     

甘地胶囊中马钱苷含量测定方法的优化

目的 建立HPLC法测定甘地胶囊中马钱苷的含量。方法 色谱柱为Waters Symmtry C₁₈柱（4.6 mm×150 mm,5 μm）;流动相为乙腈-水（13∶87）;流速1.0 ml/min;检测波长240 nm。结果 马钱苷对照品在0.030 1~3.01 μg范围内呈良好的线性关系（r=0.999 9）,平均加样回收率为99.62%,RSD为0.86%。结论 本方法简便、准确,重复性好,可用于甘地胶囊中马钱苷的含量测定。     

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.     

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.