甘肃产黄管秦艽中龙胆苦苷的鉴别与含量测定

目的对甘肃产黄管秦艽进行薄层鉴别,测定不同地区黄管秦艽的龙胆苦苷含量,以评价药材质量。方法采用薄层色谱法对黄管秦艽中的龙胆苦苷进行鉴别,并用高效液相色谱法对其进行含量测定。结果龙胆苦苷在23.5～70.5μg内线性关系良好（r=0.9993）,平均加样回收率为98.59%（RSD=1.12%,n=6）。结论薄层色谱法斑点清晰,专属性强;HPLC简便、准确、重复性好。甘肃不同地区黄管秦艽龙胆苦苷的含量有差异,但均高于中国药典2005版规定。本试验可为人工栽培秦艽、保护秦艽野生资源提供科学依据。     

甘肃产黄管秦艽中龙胆苦苷的鉴别与含量测定

目的 对甘肃产黄管秦艽进行薄层鉴别,测定不同地区黄管秦艽的龙胆苦苷含量,以评价药材质量。方法 采用薄层色谱法对黄管秦艽中的龙胆苦苷进行鉴别,并用高效液相色谱法对其进行含量测定。结果 龙胆苦苷在23.5~70.5 μg内线性关系良好(r=0.999 3),平均加样回收率为98.59%(RSD=1.12%,n=6)。结论 薄层色谱法斑点清晰,专属性强;HPLC简便、准确、重复性好。甘肃不同地区黄管秦艽龙胆苦苷的含量有差异,但均高于中国药典2005版规定。本试验可为人工栽培秦艽、保护秦艽野生资源提供科学依据。     

HPLC法测定秦艽炮制品中龙胆苦苷的含量

通过测定秦艽及秦艽炮制品中龙胆苦苷的含量,以探讨炮制方法对秦艽中龙胆苦苷的含量影响.采用高效液相色谱法,Waters C18色谱柱;流动相:甲醇水(3∶7);流速:1.0mL·min-1;检测波长:272nm.龙胆苦苷在1.104～8.280μg范围内具有良好线性关系,平均回收率为102.23%(RSD=2.9%).不同的炮制方法对秦艽中龙胆苦苷含量有一定影响.     

HPLC同步测定秦艽中龙胆苦苷和元胡中延胡索乙素的含量

目的:建立同时测定秦艽和元胡中的龙胆苦苷和延胡索素乙素含量的 RP-HPLC 分析方法。方法:采用 RP-C~(18)色谱柱,流动相:V(甲醇):V(0.1%醋酸缓冲液 pH=5.11)=30:70,等度10min,3min 梯度变成68:32,流速为1.0mL·min~(-1);紫外检测波长为230nm 和270nm。结果:龙胆苦苷和延胡索素乙素的标准曲线范围分别是4.5～449.5μg·mL~(-1)(r=0.9999,n=7)和4.9～493.5μg·mL~(-1)(r=0.9998,n=7);检测限分别是0.2245μg·mL~(-1)和0.0987μg·mL~(-1);加样回收率分别为98.9%-105.9%和97.1%～103.7%,RSD 均小于3.1%。结论:运用该方法测定龙胆苦苷和延胡索素乙素的含量稳定可靠,重现性好。     

骨筋丸胶囊中秦艽的龙胆苦苷的检测研究

目的:建立检测骨筋丸胶囊中秦艽的龙胆苦苷的方法。方法:采用薄层色谱法对秦艽进行鉴别,采用高效液相色谱法对龙胆苦苷进行含量测定,色谱柱UltimateTM XB C18,甲醇-水(30∶70)为流动相;流速0.8 mL.min-1;检测波长270 nm;进样量10μL。结果:薄层色谱中能检出骨筋丸胶囊中秦艽的龙胆苦苷;龙胆苦苷对照品在17.26～345.28μg.mL-1范围内,浓度与峰面积呈良好的线性关系,r=1.000 0,平均回收率为99.3%,RSD为2.5%(n=3)。结论:本方法简便、准确、专属性强,可以作为该制剂的质量控制方法。     

秦艽花的质量标准规范化研究

目的:建立藏药秦艽花的质量标准.方法:运用薄层色谱法对秦艽花进行定性鉴别;采用高效液相色谱法测定秦艽花中龙胆苦苷的含量,色谱柱为DIKMA Diamonsil C18(250×4.60 mm,5 μm)柱,流动相为甲醇-水(25:75),检测波长为275 nm,流速1.0 mL·min-1,柱温30 ℃.结果:薄层鉴别斑点清晰,重复性好;高效液相色谱法测定龙胆苦苷在0.912 μg～4.560 μg之间呈良好的线性关系,平均加样回收率为98.62%,RSD为1.21%.结论:该方法简单可行,重复性好,可作为藏药秦艽花的质量控制方法.     

盘龙七片质量标准的研究

目的建立盘龙七片的质量控制方法。方法用薄层色谱法对盘龙七片中的丹参、木香、当归进行定性鉴别;用HPLC法对制剂中龙胆苦苷进行含量测定。结果薄层色谱中斑点清晰,易于识别;HPLC法精密度、重复性良好。龙胆苦苷进样量在0.579~1.544μg内线性关系良好,r=0.9980,平均加样回收率98.94%(n=6),RSD为0.3%。结论该方法可有效地控制盘龙七片的产品质量。     

HPLC法测定秦艽总苷提取物中龙胆苦苷的含量

目的建立HPLC测定秦艽总苷提取物中龙胆苦苷的含量。方法采用HPLC法,以C18柱为色谱柱,以甲醇-水(25∶75)为流动相,检测波长为272nm,流速为1.0mL.min-1。结果龙胆苦苷在0.657～3.942μg范围内线性关系良好,相关系数为0.999 3;平均回收率为98.14%,RSD为0.87%。结论该方法简便、准确,结果可靠,可用于秦艽总苷提取物的质量控制。     

高效液相色谱法同时测定归芍地黄丸中4种化学成分的含量

目的建立高效液相色谱法同时测定归芍地黄丸中莫诺苷、马钱苷、芍药苷和丹皮酚的含量。方法色谱柱为Waters Symmetry C18(250 mm×4.6 mm,5μm),流动相为乙腈-0.3%磷酸溶液,梯度洗脱,柱温为35℃,流速为0.8 mL·min-1,检测波长为240 nm,外标法计算含量。结果莫诺苷进样量在0.010 48~2.62μg与峰面积线性关系良好(r=0.9999),平均加样回收率为102.8%,RSD为1.4%;马钱苷进样量在0.00868~2.17μg与峰面积线性关系良好(r=0.9999),平均加样回收率为103.6%,RSD为1.1%;芍药苷进样量在0.007 696~1.15μg与峰面积线性关系良好(r=0.9943),平均加样回收率为102.3%,RSD为2.1%;丹皮酚进样量在0.018~2.25μg与峰面积线性关系良好(r=0.9998),平均加样回收率为102.2%,RSD为1.6%。结论该方法准确、简便、可行、重复性好,可有效控制归芍地黄丸的质量。     

双波长HPLC法测定酸性龙胆合剂中龙胆苦苷和橙皮苷的含量

目的:建立双波长高效液相色谱(HPLC)法同时测定酸性龙胆合剂中龙胆苦苷和橙皮苷的含量。方法:采用HPLC法。色谱柱为Agilent ZORBAX SB-C18,流动相为甲醇-0.1%磷酸水溶液(梯度洗脱),检测波长为270 nm(龙胆苦苷)、283 nm(橙皮苷),柱温为30℃,进样量为10μl。结果:龙胆苦苷和橙皮苷的质量浓度分别在14.4~100.8μg/ml(r=0.999 7)、8.0~104μg/ml(r=0.999 7)范围内与峰面积呈良好线性关系;精密度、稳定性、重复性试验的RSD均<2%;平均加样回收率分别为99.92%、102.55%,RSD分别为0.41%、1.84%(n均为9)。结论:该方法简便、快速、灵敏,适用于酸性龙胆合剂中龙胆苦苷和橙皮苷的含量测定。     

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.