高效毛细管电泳法测定清胃黄连丸中盐酸小檗碱含量

目的建立测定清胃黄连丸中盐酸小檗碱含量的高效毛细管电泳法。方法毛细管区带电泳法,采用熔融石英毛细管柱(47cm×75μm),有效长度40 cm,缓冲溶液为pH=3.0的60 mmol/L磷酸盐溶液-甲醇(65∶35),分离电压30kV,进样时间5s,毛细管柱温25℃,紫外检测波长200 nm。结果盐酸小檗碱进样质量浓度在0.05～0.45 g/L范围内与峰面积线性关系良好(r=0.999 7),平均加样回收率为100.31%,RSD为2.53%(n=5)。结论该方法测定清胃黄连丸中盐酸小檗碱的含量灵敏、快速、结果可靠。     

差示分光光度法测定复方感冒灵片中对乙酰氨基酚的含量

目的本文选择立体异构体伪麻黄碱(1S,2S)-(-)和(1R,2R)-(+)进行CE手性分离,系统考察了分离条件的影响与优化,并建立准确、可靠、快速的分析方法.方法毛细管柱50μM(I.D.)×60cm(Ld);紫外检测波长214nm;电泳条件分离电压20kV;温度25℃;虹吸进样,高度10cm,时间3s;分离用缓冲液为25mmol/L的Tris-磷酸缓冲液,含35mmol/L的羟丙基-β-环糊精(HP-β-CD),pH2.94.结果伪麻黄碱得到的最佳分离条件分离电压20kV;温度25℃;虹吸进样,高度10cm,时间3s;紫外检测波长214nm;分离用缓冲液为25mmol/L的Tris-磷酸缓冲液,含35mmol/L的HP-β-CD,pH2.94.结论为开展此类药物对映体的研制和临床研究提供一种有效可靠的分析方法.     

土霉素及其盐酸盐含量和有关物质的分析方法

目的:采用高效液相色谱法(HPLC法)测定土霉素及其盐酸盐的含量和有关物质.方法:采用Luna C18(5 μm,250 mm×4.6 mm),以0.05 mol/L草酸铵-N,N-二甲基甲酰铵-0.2 mol/L磷酸氢二铵(60:30:10)为流动相,用氨试液调节pH值为(8.0±0.2),柱温为40℃,检测波长280 nm.结果:土霉素盐酸盐在0.15～1.5 mg/mL浓度范围内线性关系良好,r=0.999 7(n=5),土霉素与2-乙酰-2-去酰胺基土霉素等数种有关物质可得到满意的分离.结论:HPLC法简单、准确、灵敏,适用于土霉素及其盐酸盐的杂质检测和含量测定.     

毛细管电泳法测量清热化毒丸中盐酸小檗碱的含量

目的建立毛细管电泳法测量清热化毒丸中盐酸小檗碱含量的方法。方法采用甲醇溶液提取清热化毒丸样品,通过高效毛细管电泳法,测量盐酸小檗碱的含量。熔融石英毛细管柱（47cm×75m,有效长度40cm）;缓冲液体系为：60mmol／L磷酸缓冲溶液．甲醇（65：35）,pH：3．2;分离电压30KV;毛细管柱温25℃;检测波长200nm;进样时间5s。结果盐酸小檗碱在进样浓度为0．05mg／ml～0．10mg／ml内线性关系良好（r=0．9993）,平均加样加收率为103．27％,RSD为0．87％。结论该方法简便、快捷、灵敏度高、重现性好,可用于清热化毒丸中小檗碱含量的测定。     

HPCE法测定卡马西平片的含量

目的：建立高效毛细管电泳（HPCE）法测定卡马西平片含量的方法。方法：采用熔融石英毛细管（27cm×50μm）作为分离通道;以30mmol·L^-1磷酸氢二钠溶液（pH=8．0）含75mmol·L^-1十二烷基硫酸钠（SDS）为运行缓冲液;分离电压18KV;毛细管柱温30℃,检测波长280nm。压力进样10s。结果：卡马西平在5～160μg·ml^-1浓度范围内线性关系良好（r=0．9997）,平均回收率为99．9％,RSD5．8％。结论：方法简便、快速,可用于控制卡马西平片的质量。     

毛细管电泳法测定硫酸多黏菌素B中的有关物质

目的 建立一种用毛细管电泳测定硫酸多黏菌素B中有关物质的分析方法。方法 以含30mmol/L羟丙基-β-环糊精、5%异丙醇的130mmol/L三乙醇胺溶液(用磷酸调节pH至2.5)为运行缓冲液，熔融石英毛细管总长60cm，有效长度51.5cm，内径50μm，分离电压24kV，柱温25℃，进行了线性、检测限、精密度等方法学考察试验，并将该方法应用于硫酸多黏菌素B原料药及制剂的检测中。结果 实现了多黏菌素B中主要组分B1、B2、B3、B1-I与相邻杂质的分离，对比了不同来源硫酸多黏菌素B有关物质的差异。结论 本方法灵敏度较高、重复性较好，为硫酸多黏菌素B的质量控制提供了一种可行的分析方法。     

毛细管区带电泳法测定单唾液酸神经节苷脂GM_1的含量

目的建立毛细管区带电泳法分离测定单唾液酸神经节苷脂GM1 的方法。方法采用熔融的硅胶毛细管柱 (90cm× 75 μm ,有效长度为 83cm) ,以含 1 5mmol/L浕 环糊精的 2 5mmol/L硼砂缓冲液为电极缓冲液 (pH 9.4 ) ,检测波长 :2 0 0nm。结果GM1 线性范围为 0 .0 4 2～ 4 .2 3mg/ml(r =0 .9981 ) ,回收率 (n =3)分别为 98.85 % (RSD =1 .7% )、99.0 6 % (RSD =1 .1 % )、99.0 1 % (RSD =1 .2 % )。结论此法简便、快速、准确 ,适用于该药品的生产及临床应用中的质量控制     

毛细管电泳法测定一清软胶囊中盐酸小檗碱的含量

目的建立毛细管电泳法测定一清软胶囊中盐酸小檗碱含量的方法。方法采用甲醇溶液提取一清软胶囊样品,通过高效毛细管电泳法,测量盐酸小檗碱的含量。熔融石英毛细管柱（47cm×75m,有效长度40cm）;缓冲液体系为：60mmol/L磷酸缓冲溶液-甲醇（65：35）,pH=3·5;分离电压30KV;毛细管柱温25℃;检测波长200nm;进样时间5s。结果盐酸小檗碱在进样浓度为0·03018~0·08048mg/ml内线性关系良好（r=0·9998）,平均加样加收率为99·94%,RSD为1·134%。结论该方法简便、快捷、灵敏度高、重现性好,可用于一清软胶囊中小糪碱含量的测定。     

可溶性淀粉作为手性选择剂对西酞普兰的毛细管电泳手性拆分

目的:以可溶性淀粉作为手性选择剂,研究抗抑郁药西酞普兰的毛细管电泳手性拆分方法。方法:对手性选择剂的种类和浓度、缓冲溶液的浓度和pH以及分离电压等进行选择与优化。电泳条件为:石英毛细管柱内径50μm,总长56．5 cm,有效长度 44．0 cm;紫外检测波长239nm;电迁移进样10 kV×3s;温度20℃。结果:在含2．0％(w/w)可溶性淀粉、60 mmol·L-1磷酸盐 (pH 3．0)的缓冲溶液中,分离电压15 kV时,西酞普兰对映体达到基线分离,分离度为1．8。结论:采用毛细管电泳方法可以分离分析西酞普兰对映体,建立了西酞普兰对映体的毛细管电泳手性拆分方法。     

MECC法测定玄参中哈帕酯苷和安格洛苷C的含量

用胶束电动毛细管色谱法以尼泊金丙酯为内标物测定玄参中哈帕酯苷和安格洛苷C的含量。色谱条件 :75 μm × 10 0cm毛细管柱 ;分离用缓冲液为 10 0mmol/L胆酸钠含 10 %乙腈和2 0mmol/L磷酸二氢钠 ,用 2 0mmol/L硼砂调节 pH 7 5 ;运行电压2 5kV ;温度 2 5℃ ;重力进样 ,时间5s ;检测波长 2 80nm。哈帕酯苷和安格洛苷C的平均回收率分别为 (10 2 5± 3 5 ) %和 (10 2 3±2 2 ) %。本法操作简便 ,结果准确     

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.