金边瑞香滴鼻剂中瑞香素含量测定的研究

目的建立测定金边瑞香滴鼻剂中瑞香素的含量方法.方法采用高效液相色谱法,以DiamonsilTM-C18(4.6 mm×250 mm,5 μm)为色谱柱,以乙腈-水(64:36)为流动相,流速为1.0 mL·min-1,检测波长为210 nm.结果在5.08～90.19 μg·mL-1峰面积与浓度呈良好的线性关系,稳定性良好,平均加样回收率为98.94%,RSD为2.95%;重复性RSD为1.49%.结论方法精密度高、分离度良好,可作为测定金边瑞香滴鼻剂含量的方法,为质量控制提供了依据.     

HPLC同时测定瑞香狼毒中瑞香素、伞形花内酯和东莨菪内酯的含量

目的 建立HPLC同时测定瑞香狼毒中瑞香素、伞形花内酯和东莨菪内酯含量的方法。方法 样品经无水乙醇回流。采用Synergi 4u Polar-RP 80R柱（4.6 mm×250 mm,5 μm）,流动相为甲醇-1%冰醋酸溶液,等度洗脱,流速：1.0 mL·min^-1,检测波长：324 nm,柱温：30℃。结果 瑞香素在0.012~0.250 μg（r=0.999 9）、伞形花内酯在0.149~2.981 μg（r=0.999 9）、东莨菪内酯在0.012~0.239 μg（r=0.999 9）均呈良好的线性关系;瑞香素、伞形花内酯和东莨菪内酯的加样回收率分别为99.0%（RSD=0.94%）,98.7%（RSD=0.77%）和98.3%（RSD=1.16%）。结论 3种香豆素成分在35 min内达到基线分离,该方法分析时间短、稳定性和回收率良好,对瑞香狼毒药材的质量控制具有一定的参考价值。     

反相高效液相色谱法同时测定补阳还五汤中芍药苷和阿魏酸的含量

目的采用反相高效液相色谱法测定补阳还五汤中的芍药苷和阿魏酸的含量。方法固定相选用Symmetry C18柱（4.6 mm×150 mm，5 μm）；流动相为1%醋酸 甲醇（70∶30）(pH值为3.15)；流速：1.0 mL·min^-1；柱温：30 ℃；检测波长：芍药苷230 nm，阿魏酸320 nm。结果芍药苷和阿魏酸含量测定线性范围分别是4～24 μg·mL^-1，0.4～2.0 μg·mL^-1，r分别是0.999 9，0.999 8，平均加样回收率分别是101.72%（RSD＝0.27%，n＝3），104.72%（RSD＝0.46%，n＝3）。结论该检测方法简便，结果准确，可用于该方剂的质量控制。     

反相高效液相色谱法测定细梗胡枝子中槲皮素与芦丁的含量

目的建立同时分离测定细梗胡枝子中槲皮素和芦丁含量的高效液相色谱法。方法固定相：Lichrosorb C18柱（150.0 mm×4.6 mm，5 μm）；流动相：乙腈 纯化水 磷酸（47∶53∶0.2）；流速：1.0 mL·min^-1；检测波长：370 nm；柱温：40 ℃。结果槲皮素、芦丁分别在0.25～2.01 μg·mL^-1、2.54～20.32 μg·mL^-1浓度范围内线性关系良好；槲皮素、芦丁平均回收率分别为98.7%，RSD＝1.26%（n＝9）；99.2%，RSD＝1.07%（n＝9）。结论 该方法灵敏、简便、重现性好，可作为控制细梗胡枝子药材质量的方法。     

高效液相色谱法测定奥硝唑片的含量

目的建立奥硝唑片中奥硝唑的含量测定方法。方法采用高效液相色谱法，固定相：ODS-C18色谱柱(4.6 mm×150 mm，5 μm)；流动相：甲醇∶纯化水(30∶70)；流速：1.0 mL·min^-1；外标法定量；检测波长：318 mm。结果奥硝唑在20～200 μg·mL^-1范围内峰面积与浓度呈良好的线性关系，r＝0.999 9，平均回收率100.13%，RSD＝0.76%。结论该方法简便、快速、准确，适于奥硝唑片的含量测定。     

反相高效液相色谱法测定穿琥宁注射液含量

目的 建立反相高效液相色谱（RP－HPLC）法测定穿琥宁注射液中穿琥宁含量的方法。方法 色谱柱：Hypersil C18(250 mm×4.6 mm,5 μm)；流动相：0.02 mol·L^-1磷酸二氢钾溶液（pH值3.0）-乙腈-甲醇（40：10：50）；流速：1.0 mL·min^-1；柱温：25 ℃；进样量：10 μL。结果穿琥宁浓度在1.015～5.075 mg·mL 1范围内线性关系良好（r=0.999 2,n=5），精密度RSD为0.14%,平均回收率为100.5%（RSD=0.71%，n=9）。结论该方法简便、快速、准确、精密度高，可用于穿琥宁注射液的含量测定.     

反相高效液相色谱法测定唑克搽剂中盐酸克林霉素的含量

目的建立反相高效液相色谱法测定唑克搽剂中盐酸克林霉素含量的方法。方法色谱柱为Kromail C18柱(4.6 mm×250 mm，5 μm)；柱温：40 ℃；流动相为水-甲醇(21∶30)，含0.02 mol·L^-1磷酸二氢铵和0.01 mol·L^-1乙二胺四醋酸二钠，并以4 mol·L^-1磷酸溶液调节pH值至3.0；流速0.9 mL·min^-1；检测波长为367 nm。结果盐酸克林霉素在10～100 μg·mL^-1的范围内线性关系良好，r＝0.999 6(n＝6)，平均回收率为99.40 %(n＝6)，RSD为1.0 %。结论该方法简便、快速、准确，可用于唑克搽剂的质量控制。     

反相高效液相色谱法测定大青叶中邻氨基苯甲酸与丁香酸的含量

目的建立测定大青叶中邻氨基苯甲酸和丁香酸含量的反相高效液相色谱法。方法固定相：Lichrosorb C18色谱柱(4.6 mm×150 mm ，5 μm)；流动相：乙腈-水-磷酸(18∶82∶0.3)；检测波长:272 nm；流速：0.8 mL·min^－1；柱温：30 ℃；进样体积：10 μL。结果邻氨基苯甲酸、丁香酸分别在12.7～127.0和5.10～51.0 μg·mL^－1浓度范围内线性关系良好；邻氨基苯甲酸的平均回收率为98.7%(RSD＝1.0%)；丁香酸的平均回收率为99.0%(RSD＝1.2%)。结论该方法灵敏、快速，准确可靠。     

高效液相色谱法测定菝葜醋酸乙酯提取物中白藜芦醇的含量

目的建立高效液相色谱法测定菝葜醋酸乙酯提取物中白藜芦醇含量的方法。方法Zirchrom Kromasil C18 色谱柱(4.6 mm×250 mm，5 μm)；流动相：乙腈-水(30∶70)；流速：1.0 mL·min^-1；柱温：室温；检测波长303 nm。结果白藜芦醇对照品线性范围18.8～94.0 μg·mL^-1，r＝0.999 6(n＝5)，样品平均回收率为101.10 %，RSD＝0.64 %(n＝5)，菝葜醋酸乙酯提取物中白藜芦醇的平均含量为29.59 μg·mg^-1。结论该方法简便、快捷、重现性好，为菝葜醋酸乙酯提取物的质量控制提供依据。     

复方双嘧达莫缓释片中阿司匹林和双嘧达莫的含量测定

目的建立同时测定复方双嘧达莫缓释片中阿司匹林和双嘧达莫含量的方法。方法采用反相高效液相色谱法，色谱柱：Alltech C18(4.6 mm×150 mm，5 μm)；流动相：甲醇-0.3%二乙胺水溶液-冰醋酸(45∶55∶4)；检测波长：235 nm；流速：1.2 mL·min^-1；柱温：30℃。 结果阿司匹林在635～101.60 μg·mL^-1范围内，峰面积与其浓度呈良好线性关系(r＝0.999 9，n＝6)，平均回收率为99.87%，RSD＝0.61%；双嘧达莫在18.7～299.2 μg·mL^-1范围内，峰面积与其浓度呈良好线性关系(r＝0.999 9， n＝6)，平均回收率为100.29%，RSD＝0.40%。3批自制复方双嘧达莫缓释片中阿司匹林和双嘧达莫相当于标示量的百分含量分别为：100.5%，100.4%，99.5%和100.9%，99.34%，100.3%。结论该法具有准确、简便、快速、灵敏且重现性好的特点，可用于复方双嘧达莫缓释片中阿司匹林和双嘧达莫含量的同时测定。     

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.