HPLC同时测定珠子草中没食子酸、短叶苏木酚和鞣花酸的含量

目的 建立同时测定珠子草中没食子酸、短叶苏木酚和鞣花酸的HPLC法,并对珠子草该3种成分进行含量测定。方法 色谱柱：Shimazu C₁₈(150 mm×4.6 mm,5 μm);流动相：0.1%磷酸(A)-乙腈(B)梯度洗脱,流速为0.8 mL·min^-1;柱温：室温;检测波长：270 nm;进样量10 μL。结果 没食子酸、短叶苏木酚和鞣花酸含量分别在0.6~9.6 μg、0.525~8.4 μg、0.475~7.6 μg内与峰面积呈良好的线性关系。没食子酸的平均含量为0.196 2%,短叶苏木酚为0.518 2%,鞣花酸为0.411 0%。结论 本方法操作简便,准确度高,可用于珠子草中没食子酸、短叶苏木酚和鞣花酸3种成分含量的测定。     

石榴叶鞣质中短叶苏木酚在大鼠体内药代动力学变化

目的建立测定短叶苏木酚血药浓度的高效液相色谱方法,探讨大鼠ig石榴叶鞣质后体内短叶苏木酚动力学变化。方法色谱条件依利特Hypersil色谱柱;流动相为乙腈-5mmol·L-1磷酸二氢钾溶液(pH25;86∶14,V/V);流速10ml·min-1;紫外检测波长为276nm,以短叶苏木酚峰面积定量。结果短叶苏木酚在176~880μg·L-1内线性良好,回归方程为^Y=393E5X+182E3(n=5),相关系数r2=09994,血浆中最低检测浓度为176μg·L-1。其352,176,880μg·L-13个浓度的回收率>85%,日内日间变异<7%。大鼠ig石榴叶鞣质后短叶苏木酚体内吸收、分布及消除均较快,符合二室开放模型。结论短叶苏木酚可以部分的反映了石榴叶鞣质的药代动力学特征。     

RP-HPLC法同时测定叶下珠中没食子酸、柯里拉京和短叶苏木酚的含量

目的建立反相高效液相色谱法同时测定叶下珠中没食子酸、柯里拉京和短叶苏木酚的含量。方法采用Kromasil C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-体积分数0.1%磷酸水溶液梯度洗脱,流速1.0 mL.min-1,检测波长为280 nm,柱温30℃。结果没食子酸、柯里拉京和短叶苏木酚的质量浓度分别在5.300～106.7 mg.L-1(r=0.999 8)、2.00～40.6 mg.L-1(r=0.999 7)、0.270～5.42 mg.L-1(r=0.999 7)内与峰面积呈良好的线性关系。没食子酸、柯里拉京和短叶苏木酚的平均加样回收率(n=9)分别为97.9%、101.7%、100.2%,RSD分别为1.8%、1.8%、2.7%。结论该分析方法准确可靠,重复性好,为更好地控制叶下珠药材的质量提供方法。     

HPLC法同时测定紫果西番莲叶中荭草素、异荭草素与牡荆素的含量

目的:建立同时测定紫果西番莲叶中荭草素、异荭草素与牡荆素含量的方法。方法:采用高效液相色谱法。色谱柱为Inertsil C18(250mm×4.6mm,5μm),流动相为乙腈-0.1%磷酸溶液(梯度洗脱),检测波长为350nm,流速为1mL·min-1,柱温为30℃。结果:异荭草素、荭草素与牡荆素的检测浓度分别在0.015～0.150mg·mL-1(r=0.9998)、0.012～0.120mg·mL-1(r=0.9998)、0.012～0.120mg·mL-1(r=0.9994)范围内与各自峰面积积分值呈良好线性关系;平均回收率分别为99.04%(RSD=0.80%,n=6)、99.30%(RSD=1.03%,n=6)、98.92%(RSD=1.11%,n=6)。结论:本方法简便、准确,可为紫果西番莲叶的进一步开发利用提供质量控制依据。     

贵州产黄珠子草总黄酮毒性及抗CCl4、AAP中毒小鼠肝损伤实验

黄珠子草为大戟科叶下珠属(Phyllanthus)植物,贵州产叶下珠属植物黄珠子草(Phyllanthus Virgatus Forst．f．)广泛分布于兴义、兴仁、织金、贞丰等地。我们采用贵州产黄珠子草已进行其总黄酮的提取分离方法与含量测定,但资料查新未见有关贵州产黄珠子草总黄酮毒性与抗肝损伤等方面的研究报道。为此我们特进行了贵州产黄珠子草总黄酮毒性及抗CCl4、AAP中毒小鼠肝损伤实验,现将其研究结果报告如下。     

HPLC法测定赶黄草根、茎、叶中6种成分成分

摘要：目的:比较不同产地赶黄草根、茎、叶中6种成分的含量,为该药材资源的综合开发利用提供科学依据。方法:采用Shim-pack GIST C18色谱柱（250 mm×4.6 mm, 5μm）,流动相为乙腈-0.05%磷酸水溶液,梯度洗脱,检测波长:340 nm,流速:1.0 ml·min-1,柱温:35℃,进样量:20μl。采用SPSS 22.0、SIMCA 14.0统计软件对赶黄草根、茎、叶中6种成分的含量进行主成分分析与聚类分析。结果:芦丁、没食子酸、槲皮素、原儿茶酸、芹菜素、山柰酚质量浓度分别在0.028 0～0.570 0 mg·ml-1（r=0.999 7）、0.012 0～0.246 0 mg·ml-1（r=0.998 3）、0.034 0～0.682 0 mg·ml-1（r=0.999 9）、0.084 0～1.683 0 mg·ml-1（r=0.999 5）、0.007 0～0.144 0 mg·ml-1（r=0.997 9）和0.010 0～0.203 0 mg·ml-1（r=0.998 6）范围内与峰面积呈良好线性关系,平均加样回收率在98.4%～100.0%,RSD在0.04%～1.42%之间（n=6）。聚类分析将赶黄草按根、茎和叶分为2大类,其中赶黄草叶与其余2个部位的差异较明显,主成分分析出不同药用部位赶黄草药材最佳入药部位为叶。结论:赶黄草的根、茎和叶中化学成分差异较大,建议在调配以赶黄草入药的方剂过程中应综合考虑饮片中根、茎和叶的比例,更好地提高药物疗效。     

HPLC法测定山奈酚胃漂浮缓释片中主药含量

目的:建立高效液相色谱法测定山奈酚胃漂浮缓释片中主药含量的方法。方法:色谱柱为Hypersil ODS C18,流动相为甲醇-0.4%醋酸溶液(48∶52),流速为0.8mL·min-1,检测波长为360nm,柱温为45℃。结果:山奈酚检测浓度线性范围为5.0～40.0μg·mL-1(r=0.9997);方法回收率为100.29%,RSD=1.77%(n=6)。结论:本方法灵敏、准确、专属性强,可用于山奈酚胃漂浮缓释片中主药含量的测定。     

HPLC-MS法测定双黄连口服液中木犀草苷和绿原酸的含量并评价二者对成品质量的影响

目的:建立测定双黄连口服液中主要成分木犀草苷含量的方法,并探讨木犀草苷和绿原酸对成品质量控制的影响。方法:木犀草苷含量测定采用高效液相色谱-质谱联用法。色谱柱为Agilent HC-C18柱,流动相为0.2%磷酸(A)-乙腈(B)(梯度洗脱),流速为1mL·min-1,检测波长为350nm,进样量为10μL,柱温为25℃;绿原酸的含量测定采用2010年版《中国药典》(一部)双黄连口服液项下方法。通过测定9批双黄连口服液样品和4个模拟样品中木犀草苷和绿原酸的含量分析二者对成品质量的影响。结果:木犀草苷检测浓度在3.9～39.0μg·mL-1范围内与峰面积积分值呈良好线性关系(r=0.9999),平均加样回收率为99.5%,RSD=3.6%。9批双黄连口服液中木犀草苷的含量为5.56～30.20μg·mL-1,有较大差异;绿原酸的含量为0.71～0.94μg·mL-1,差异不大。4个模拟样品中木犀草苷的含量为0～33.28μg·mL-1,有较大差异;绿原酸的含量为1.07～1.23μg·mL-1,差异不大。结论:仅测定绿原酸来表征双黄莲口服液中金银花的含量有失准确、专属和有效,建议在双黄连口服液质量标准中增加木犀草苷的含量测定。     

樱桃叶中黄酮类成分的定性定量研究及体外抗氧化活性初步评价

目的:建立樱桃叶中黄酮类成分的定性定量方法,并初步评价其体外抗氧化活性。方法:药材经水解后提取总黄酮;紫外分光光度(UV)法测定总黄酮含量;薄层色谱(TLC)法检测槲皮素和山柰酚的存在与否;高效液相色谱(HPLC)法测定槲皮素与山柰酚的含量;Fenton反应法评价抗氧化活性。结果:UV法芦丁的检测浓度在11.0～110.0μg·mL-1范围内与吸光度呈良好线性关系(r=0.9998),平均加样回收率为98.3%(RSD=1.3%,n=6);TLC可清晰检出槲皮素与山柰酚;HPLC法槲皮素与山柰酚的检测浓度分别在37.5～1200.0ng·mL-(1r=0.9997)、62.5～2000.0ng·mL-(1r=0.9994)范围内与各自峰面积积分值呈良好线性关系,平均加样回收率分别为99.8%(RSD=3.4%,n=9)、100.0%(RSD=1.9%,n=9);樱桃叶总黄酮提取液具有一定抗氧化能力,并呈量-效关系。结论:该方法准确、可靠、重复性好,可作为樱桃叶的质量控制方法。     

HPLC法测定藿香正气胶囊中厚朴酚与和厚朴酚的含量

目的测定藿香正气胶囊中厚朴酚与和厚朴酚的含量.方法采用HPLC法.色谱柱:采用Thermo 1254133T色谱柱(250×4.6mm,5μm);流动相:甲醇-水(75∶25);流速:1.0mL·min-1;检测波长:294nm.结果厚朴酚平均回收率为99.81%,RSD=0.3%(n=5);和厚朴酚平均回收率为100.14%,RSD=0.8%(n=5).结论方法简单易行,结果准确,可靠,适用于本品的含量测定.     

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.     

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.