高效液相色谱法测定天麻中7种成分含量

目的 建立采用高效液相色谱法测定天麻中7个成分含量的方法。方法 天麻药材粉碎过三号筛,用60%甲醇溶液涡旋、超声提取,,然后过0.45 μm滤膜过滤,采用C₁₈（4.6 mm×250 mm,5 μm）色谱柱,以乙腈（A）-0.05%磷酸水溶液（B）为流动相,梯度洗脱,检测波长 220 nm,流速 1.0 mL·min^-1,柱温 35 ℃测定,标准曲线法定量。结果 7种成分在相应的范围内线性关系良好,r≥0.999;回收率(n=6)均在为92.1%~103.9%之间,其相对偏差为RSD=0.75%~1.65%;并对25批样品进行了检测。结论 本法适用于天麻中腺苷、天麻素、对羟基苯甲醇、巴利森苷A、巴利森苷B、巴利森苷C、巴利森苷E含量的测定。     

HPLC同时测定坤泰胶囊中毛蕊花糖苷、芍药苷和黄芩苷含量

目的 建立HPLC同时测定坤泰胶囊中毛蕊花糖苷、芍药苷和黄芩苷含量的方法，为完善现有质量标准提供参考。方法 采用Phenomsil C₁₈（4.6 mm×250 mm，5 μm）色谱柱；以乙腈为流动相A，以0.1%乙酸为流动相B，采用梯度洗脱；流速为1.0 mL·min^-1；柱温为35℃；毛蕊花糖苷的检测波长为334 nm，芍药苷检测波长为230 nm，黄芩苷的检测波长为280 nm。结果 毛蕊花糖苷在3.27~32.68 μg·mL^-1内线性关系良好，平均回收率为98.4%，RSD为0.68%（n=6）；芍药苷在17.65~176.51μg·mL^-1内线性关系良好，平均回收率为99.2%，RSD为1.08%（n=6）；黄芩苷在48.78~487.77 μg·mL^-1内线性关系良好，平均回收率为97.7%，RSD为0.87%（n=6）。结论 该方法简便、快捷、结果准确、重复性好，可应用于坤泰胶囊的质量控制。     

HPLC-ELSD法测定复胃散胶囊中黄芪甲苷的含量

目的 建立高效液相色谱-蒸发光散射检测器法测定复胃散胶囊中黄芪甲苷的含量。方法 采用Agilent 1200高效液相色谱仪和Waters XSELECT C₁₈色谱柱（4.6 mm×250 mm,5 μm）,流动相为乙腈-水（32:68）,流速为1.0 mL·min^-1,进样量为20 μL,蒸发光散射检测器（漂移管温度为70 ℃,载气流速为2.0 L·min^-1）。结果 黄芪甲苷在0.050 5～1.011 mg·mL^-1的范围内呈良好的线性关系,标准曲线为lgA=1.3555lgC+3.277 6,（r=0.999）;精密度和重复性的RSD分别为1.2%和1.6%;平均回收率为96.1%,RSD为1.7%。结论 该方法简便准确、快速、方便、精密度高、重复性好,可用于复胃散胶囊中黄芪甲苷的含量测定。     

高效液相色谱法测定鼻炎灵胶囊中黄芩苷含量

目的 建立高效液相色谱法测定鼻炎灵胶囊中黄芩苷的含量。方法 色谱柱为Waters XBridge C₁₈柱（4.6 mm×250 mm,5 μm）,流动相为乙腈-0.8%甲酸（25：75）,检测波长276 nm,流速1.0 ml/min,柱温30℃,进样量10 μl。结果 黄芩苷在1.25~40 μg/ml范围内（r=0.999 9）呈良好的线性关系,精密度实验中RSD均小于2%,加样回收率在95%~100%之间。结论 该测定方法简便、准确,分离效果好,可用于鼻炎灵胶囊的质量控制。     

HPLC法测定肌瘤化消颗粒中淫羊藿苷和丹参酮ⅡA

目的 建立测定肌瘤化消颗粒中淫羊藿苷和丹参酮II_A的HPLC法。方法 采用高效液相色谱法,Diamonsil^TM C₁₈色谱柱（250 mm×4.6 mm,5 μm）;流动相：乙腈-水,梯度洗脱;检测波长为270 nm;柱温为40℃;体积流量为1.0 mL/min;进样量10 μL。结果 淫羊藿苷在7.5～50 μg、丹参酮II_A在3～20 μg与峰面积的线性良好（r=0.999 9）。平均回收率分别为100.2%、100.1%,RSD值分别为0.9%、1.3%（n=9）。结论 本法操作简便,重现性好,可有效控制肌瘤化消颗粒的质量。     

甘地胶囊中马钱苷含量测定方法的优化

目的 建立HPLC法测定甘地胶囊中马钱苷的含量。方法 色谱柱为Waters Symmtry C₁₈柱（4.6 mm×150 mm,5 μm）;流动相为乙腈-水（13∶87）;流速1.0 ml/min;检测波长240 nm。结果 马钱苷对照品在0.030 1~3.01 μg范围内呈良好的线性关系（r=0.999 9）,平均加样回收率为99.62%,RSD为0.86%。结论 本方法简便、准确,重复性好,可用于甘地胶囊中马钱苷的含量测定。     

HPLC同时测定肺宁制剂中4种成分的含量

目的 建立HPLC同时测定肺宁颗粒、肺宁胶囊和肺宁片中新绿原酸、绿原酸、隐绿原酸和金丝桃苷4种成分的含量。方法 采用Waters XBridge^TMC₁₈色谱柱（4.6 mm×250 mm,5 μm）,流动相为乙腈-0.4%磷酸水溶液,梯度洗脱,流速1.0 mL·min^-1;检测波长327,353 nm;柱温30℃。结果 4种成分在各自范围内线性关系良好（r>0.9990）,平均加样回收率96.1%~104.7%,RSD为0.4%~1.6%。结论 该方法准确、可靠,重复性好,可用于肺宁制剂的质量控制。     

HPLC测定绞股蓝中七叶胆苷XLVI和人参皂苷Rb3含量

目的 建立HPLC测定绞股蓝中七叶胆苷XLVI和人参皂苷Rb₃含量的方法。方法 采用Ultimate XB-C₁₈色谱柱（250 mm×4.6 mm，5 μm），以乙腈（A）-水（B）线性梯度洗脱，检测波长203 nm，流速1 mL·min^-1，柱温30℃。结果 七叶胆苷XLVI在3.30~39.62 μg·mL^-1范围内线性良好（r²=0.999 7），平均回收率为113%，RSD为1.84%；人参皂苷Rb₃在3.27~39.26 μg·mL^-1范围内线性良好（r²=0.999 7），平均回收率为102%，RSD为2.82%。结论 该方法有较好的分离效果，准确性、精密度和重复性良好，为绞股蓝的研究和质量控制提供了科学依据。     

白麻叶和罗布麻叶的化学成分与抗炎活性比较研究

目的 比较研究白麻Apocynum pictum叶和罗布麻Apocynum venetum叶的化学成分及抗炎活性差异。方法 取白麻叶和罗布麻叶,20倍量60%乙醇溶液回流提取 2 次 ,每次 1.5 h ,合并提取液,浓缩、干燥,即得白麻叶提取物（APLE）、罗布麻叶提取物（AVLE）;以每毫升药液0.03 g药材的浓度过HPD300大孔树脂柱,水洗除杂后以60%乙醇溶液洗脱,收集洗脱液,浓缩、干燥,即得白麻叶精制物（APLP）、罗布麻叶精制物（AVLP）。利用UPLC/Q-TOF/MS鉴定白麻叶和罗布麻叶提取物及精制物的化学成分,进而以HPLC检测白麻苷、芦丁、异槲皮苷、金丝桃苷和紫云英苷的含量。在进行急性毒性实验确定最大耐受剂量的基础上,采用小鼠棉球肉芽肿模型考察4种样品对小鼠肉芽肿指数、抑制率和肾上腺指数的影响,并检测血清组胺、5-羟色胺和前列腺素E₂（PGE₂）水平。结果 以UPLC/Q-TOF/MS从4种样品中鉴定出化学成分97个,其中白麻叶和罗布麻叶的共有化学成分82个,主要是黄酮、黄酮糖苷和黄烷酮。HPLC检测结果显示,APLE、APLP中的白麻苷质量分数分别为 2.43%和 11.98%,罗布麻样品中未检出白麻苷,但 AVLP中芦丁、异槲皮苷、金丝桃苷和紫云英苷的质量分数分别是APLP的30.37、1.75、8.64、1.58倍。动物实验表明,与模型组比较,1.50、0.75 g·kg^-1的APLP可显著降低小鼠棉球肉芽肿指数（P＜0.05）,抑制率分别为 25.79%、21.75%;1.50 g·kg^-1剂量可显著降低血清组胺和 5-羟色胺水平（P＜0.05）,0.75 g·kg^-1剂量可显著降低 5-羟色胺水平（P＜0.01）;APLE、APLP 下调 PGE₂水平,差异不显著;AVLE、AVLP 显著升高PGE₂水平（P＜0.05）。结论 白麻叶和罗布麻叶的化学成分同中有异,相同方法制备的样品在抗炎活性上有较为明显的差别,其中APLP的抗炎活性最强,作用机制可能与调节血管活性胺的释放相关。     

HPLC-DAD同时测定益心通胶囊中6种活性成分的含量

目的 建立HPLC同时测定益心通胶囊中葛根素、龙胆苦苷、阿魏酸、毛蕊花糖苷、丹酚酸B和丹皮酚6种活性成分含量的方法。方法 采用XSELECT^TM HSS C₁₈色谱柱,流动相为乙腈（A）-0.2%磷酸水溶液（B）,梯度洗脱;柱温：30℃;流速：1.0 mL·min^-1;检测波长：阿魏酸、毛蕊花糖苷和丹酚酸B为220 nm,葛根素为250 nm,龙胆苦苷和丹皮酚为275 nm。结果 葛根素、龙胆苦苷、阿魏酸、毛蕊花糖苷、丹酚酸B和丹皮酚的线性范围分别为7.56~113.4 μg·mL^-1（r=0.999 8）,4.36~65.4μg·mL^-1（r=0.999 7）,1.18~17.7 μg·mL^-1（r=0.999 3）,1.90~28.5 μg·mL^-1（r=0.999 4）,4.48~67.2 μg·mL^-1（r=0.999 3）和11.7~175.5 μg·mL^-1（r=0.999 7）,平均加样回收率分别为98.7%,97.8%,97.6%,98.6%,99.0%,98.7%,RSD分别为1.0%,1.3%,1.4%,1.1%,1.2%,1.3%。结论 本法专属性强,结果准确,重现性好,可用于益心通胶囊的质量控制。     

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.     

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.     

Alzheimer’s disease – current trends in basic and clinical research. Highlights from the 16th ECNP

Advances in the molecular biological knowledge of neuronal nicotinic acetylcholine receptors (nAChRs) have led to a growing interest by the pharmaceutical industry in the development of novel compounds that selectively modulate nAChR function. The ability of (-)-nicotine, an activator of nAChRs, to enhance attentional aspects of cognition in animals and humans, to exert neuroprotective and anxiolytic-like effects, and presumably to mediate the negative correlation between smoking and Alzheimer's (and Parkinson's) Disease, has focused interest on the potential therapeutic utility of modulators of nAChR function for treatment of some of the deficits associated with these progressive, neurodegenerative conditions. Numerous compounds are known which activate nAChRs and which might serve as lead compounds toward the development of such agents. The pharmacologic diversity of neuronal nAChR subtypes suggests the possibility of developing selective compounds which would have more favourable side-effect profiles than existing agents. This broader class of agents, collectively called cholinergic channel modulators (ChCMs), is anticipated to encompass compounds which would have more favourable side-effect profiles than existing agents, which generally exhibit low selectivity. This selectivity may be achieved by preferentially activating some subtypes of nAChRs (i.e., Cholinergic Channel Activators, ChCAs) or inhibiting the function of other subtypes (Cholinergic Channel Inhibitors, ChCIs). An overview of the biology of nAChRs and the rationale for the use of ChCMs for the treatment of dementia related to neurodegenerative diseases are presented, followed by a discussion of lead compounds and compounds under consideration for clinical evaluation.     

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.