十二指肠腺腺瘤合并肠套叠影像学诊断及文献复习１例

目的：提供一种琥珀酸美托洛尔缓释片的体外释放度测定方法。方法以pH6．8磷酸盐缓冲液为溶出介质,转速100 rpm,以高效液相色谱法测定含量,色谱柱为venusil MPC18（250 mm ×4．6 mm,5μm）,流动相为pH 3．5的磷酸盐缓冲液－乙腈（75∶25）,检测波长为274 nm,流速：1．0 mL· min－1。结果 A＝9．2322C＋7．3634（r＝0．9999）,琥珀酸美托洛尔含量测定浓度在20～140 mg· L－1的范围内线性关系良好;自制制剂与进口制剂具有相似的体外释放特征。结论该法操作简便、准确、重现性好,适合琥珀酸美托洛尔缓释片的释放度测定。     

RP-HPLC测定琥珀酸美托洛尔缓释片的含量及有关物质

目的：建立琥珀酸美托洛尔缓释片含量及有关物质的RP－HPLC方法。方法以十八烷基硅烷键合硅胶作为填充剂ZORBAX SB－C18（4．6 mm ×250 mm,5μm）,以乙酸铵缓冲液（3．9 g的乙酸铵溶解于810 mL的水中,加入10．0 mL的冰乙酸,2．0 mL的三乙胺,3．0 mL的磷酸）—乙腈＝82∶18,流速1．0 mL· min－1,检测波长275 nm,进样量10μL。结果琥珀酸美托洛尔在20．00～120．02 mg· L－1浓度范围内线性关系良好,检测限为0．4 ng,定量限为1．2 ng,回收率为100．75％（ RSD＝0．67％）,测定样品含量为99．8％,有关物质均小于0．2％。结论该方法快速,简单,稳定,重现性好,可作为琥珀酸美托洛尔缓释片的含量及有关物质的检测方法。     

高效液相色谱法测定那格列奈胶囊的有关物质

目的：建立高效液相色谱法测定那格列奈胶囊有关物质的方法。方法采用AlltimaTM C18柱（250 mm ×4．6 mm,5μm）色谱柱,以磷酸盐缓冲液（ pH＝3．0）—乙腈为流动相进行梯度洗脱,流速为1．0 mL· min－1,柱温为30℃,检测波长为210 nm,进样量为20μL。结果高效液相色谱法测定有关物质的线性范围均为0．5～10．0 mg· L－1,相关系数均大于0．999（n＝6）。结论该方法简单、精确,有关物质的分离度较好,可以作为那格列奈胶囊有关物质的测定方法。     

对《中国药典》青霉素V钾片含量测定方法中流动相的改进

目的：改进青霉素V钾片含量测定的方法。方法：色谱条件：Inertis ODS－SP C18柱（150mm×4．6mm,5μm）;流动相为A-B（60：40）[A：pH3．5磷酸盐缓冲液（取0．5m01·L^-1磷酸二氢钾溶液,用磷酸调节pH至3．5）－乙腈．水（10：30：60）;B：pH3．5磷酸盐缓冲液．乙腈－水（10：55：35）];流速为1．0ml·min^-1;检测波长268nm;柱温：室温;进样量：10tzl。结果：青霉素V钾在0．0329—0．8216mg·ml“范围内呈良好线性关系（r=0．9999）;平均回收率99．9％,RSD为0．6％（n=9）。结论：此法重复性好,结果准确,可用于青霉素V钾、青霉素V钾片及胶囊的含量测定。     

复方单硝酸异山梨酯缓释片中单硝酸异山梨酯的释放度测定

目的建立高效液相色谱法,测定复方单硝酸异山梨酯缓释片中单硝酸异山梨酯的释放度。方法以pH=5．0的磷酸盐缓冲液250mL为溶剂．转速为100r／min。以高效液相色谱法测定含量,色谱柱为LunaODS C18（250mm×4．6mm,5μm）,流动相为1％醋酸溶液（加0．1％三乙胺）-甲醇（55：45）,检测波长230nm,流速1．0mL／min。结果单硝酸异山梨酯质量浓度线性范围为19．66～314．56μg／mL（r=0．9999）,平均回收率为100．27％,RSD=1．78％（n=9）;体外释放符合Higuchi方程,与国外对照样品一致。结论该方法简便、准确,可作为复方单硝酸异山梨酯缓释片的释放度测定方法。     

非洛地平-美托洛尔缓释片处方优化及体外释放一致性评价

目的 优化非洛地平-美托洛尔缓释片的处方，并评价其与市售制剂体外释放的一致性。方法 采用HPLC测定非洛地平-美托洛尔缓释片中非洛地平及美托洛尔的释放度；以体外释放度为评价指标，重点考察了固体分散体、微丸以及片芯中关键处方因素对非洛地平/美托洛尔释放行为的影响，进一步优化处方。结果 微丸组成、微丸粒径、微丸衣膜中致孔剂用量、微丸增重以及片芯中阻滞剂用量均影响药物释放；处方优化后自制的非洛地平-美托洛尔缓释片与市售制剂在0.3% SDS水溶液、含0.3% SDS的pH 4.0的柠檬酸缓冲液、含0.3% SDS的pH 6.8的磷酸盐缓冲液、含0.3% SDS的0.1 mol·L^-1 HCl中的体外释放行为一致。结论 自制非洛地平-美托洛尔缓释片与市售制剂的体外释放行为一致。     

罗红霉素缓释胶囊含量和释放度测定方法研究

目的：建立罗红霉素缓释胶囊含量和释放度测定方法。方法：采用高效液相色谱法,色谱柱为ZORBAX SB-C18（4.6 mm ×150 mm,5μm）,0.067 mol· L-1磷酸二氢铵溶液（三乙胺含量0.3％,调pH值至7.5）-乙腈（60∶40）为流动相,检测波长210 nm,用外标法计算罗红霉素缓释胶囊含量;释放度测定以磷酸盐缓冲液（pH 6.8）为溶剂,溶出2,4,8 h时取样测定。结果：含量测定在0.22～2.00 mg· mL-1（ R2＝0.9999）浓度范围内呈良好的线性关系,平均回收率为101.50％（ RSD＝1.07％）;样品在2,4,8 h的释放率分别相应为标示量的15％～45％、40％～70％和70％以上。结论：该方法简便、准确,适用于罗红霉素缓释胶囊含量和释放度的测定。     

头孢氨苄缓释片含量测定方法的改进

目的建立头孢氨苄缓释片含量测定最佳条件的高效液相色谱方法。方法色谱柱为Wondasil C18（4．6mm×250mm,5μm）分析柱。以磷酸盐缓冲液（pH6．8）-甲醇（80：20）为流动相,流速1．0ml／min,检测波长为260nm。结果头孢氨苄浓度在3．92～58．85μg/ml范围内与峰面积呈现良好关系,平均回收率99．6％,RSD为1．1％（n=5）。结论本法准确度高,专属性强,操作简便,可用于头孢氨苄缓释片的含量测定。     

注射用美洛西林钠的HPLC测定

高效液相色普外标法测定注射用美洛西林钠的含量。采用Shim-PackCLC－ODS柱，以混合磷酸盐缓冲液－乙腈（65：35，pH＝6．1）为流动相，检测波长为298nm，线性范围为3．7μg（r＝0．9999），回收率为99．9％－100．0％，RSD小于0．54％。     

琥珀酸美托洛尔缓释片体外加速释放度试验方法的研究

目的：建立琥珀酸美托洛尔缓释片（商品名：倍他乐克）的加速释放度试验方法,考察琥珀酸美托洛尔缓释片的加速释放度和常规释放度曲线的相关性。方法：通过提高水浴温度,增加桨板转速和改变释放介质等加速条件将常规释放度试验加速完成。采用时间刻度相关性评价法筛选出最佳加速释放条件,并评价常规释放条件和加速释放条件试验结果的相关性。结果：加速释放方法将琥珀酸美托洛尔缓释片的释放度测定时间由20 h缩短为4.5 h,且与常规释放条件测定结果相关性良好。结论：加速释放度试验可以大大节约用于缓控释制剂研发及质量控制的时间和资源。     

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.