高效液相色谱法测定六味地黄胶囊中芍药苷含量的实验研究

目的建立六味地黄胶囊中芍药苷含量的高效液相色谱法（HPLC）测定方法。方法采用Kromasil色谱柱,芍药苷以乙腈—水（含0.08%磷酸、0.08%三乙胺）为流动相,检测波长为230nm。结果芍药苷的线性范围为30.52～305.2μg/ml（r=0.9999）,平均回收率为100.76%,相对标准偏差（RSD）为1.14%（n=9）。结论 HPLC操作简便、准确、重现性好,能有效控制六味地黄胶囊中芍药苷的质量。     

HPLC法同时测定胃气痛片中芍药苷与橙皮苷的含量

目的：采用HPLC法同时测定胃气痛片中芍药苷与橙皮苷的含量。方法采用Hypersil ODS2（150 mm×4.6 mm,5μm）色谱柱;流动相为乙腈-0.1%磷酸水溶液梯度洗脱,流速为1.0 mL·min-1;检测波长为230 nm;进样量为10μL;柱温为25℃。结果芍药苷在0.1652-1.1564μg范围内呈良好的线性关系（r=0.9999）,橙皮苷在0.1698-1.1886μg范围内呈良好的线性关系（r=0.9994）。芍药苷的平均加样回收率为100.5%（n=6）,RSD=1.8%;橙皮苷的平均加样回收率为98.9%（n=6）,RSD=1.1%。结论该方法操作简便、准确、稳定,适用于胃气痛片中芍药苷与橙皮苷的含量测定。     

基于HPLC多指标成分联合化学计量学的阑尾清解汤的综合质量评价

摘要：目的:建立HPLC法同时检测阑尾清解汤中氧化芍药苷、芍药内酯苷、芍药苷、连翘酯苷B、连翘酯苷A、连翘苷、木犀草苷、木犀草素和菊苣酸的含量,并结合化学计量学构建其质量评控体系。方法:采用Venusil XBP C18（250 mm×4.6 mm, 5μm）色谱柱,流动相为乙腈-0.2%磷酸,梯度洗脱;检测波长分别为230 nm（检测氧化芍药苷、芍药内酯苷和芍药苷）、275 nm（检测连翘酯苷B、连翘酯苷A和连翘苷）和350 nm（检测木犀草苷、木犀草素和菊苣酸）;运用聚类分析（CA）、主成分分析（PCA）和偏最小二乘法-判别分析（PLS-DA）对检测结果进行综合评价。结果:9种成分分别在各自范围内线性关系良好（r≥0.999 2）;平均加样回收率在96.90%～100.09%（RSD≤1.62%）之间。通过化学计量学分析,变量重要性投影（VIP）＞1的4个成分,即连翘苷（VIP=1.591）、连翘酯苷A（VIP=1.441）、木犀草素（VIP=1.089）和芍药苷（VIP=1.074）是影响阑尾清解汤产品质量的差异性标志物。结论:所建立的HPLC法多指标成分定量控制及化学计量学模式识别专属性强,可用于阑尾清解汤质量控制和综合评价。     

HPLC法同时测定麻仁丸中芍药苷、柚皮苷及橙皮苷的含量

目的：增加麻仁丸的含量测定方法,建立同时检测芍药苷,柚皮苷及橙皮苷的测定方法。方法：采用C18色谱柱;水-乙腈为流动相,进行梯度洗脱;流速1.0mL·min-1;检测波长230nm。结果：线性范围：芍药苷0.03075～0.2050g·L-1（r2=0.9997）,柚皮苷0.1148～0.7650g·L-1,r2=0.9997,橙皮苷0.01275～0.08500g·L-1（r2=0.9996）;平均回收率：芍药苷99.4%,RSD=0.9%（n=6）,柚皮苷99.7%,RSD=1.2%（n=6）,橙皮苷98.6%,RSD=2.0%（n=6）。结论：该方法操作简便、准确,重复性好,可用于麻仁丸的质量控制。     

HPLC双波长法同时测定消石利胆胶囊中芍药苷、橙皮苷、黄芩苷和大黄酚的含量

目的:建立HPLC双波长法同时测定消石利胆胶囊中芍药苷、橙皮苷、黄芩苷和大黄酚的含量。方法:采用Inertsil ODS-3 C₁₈色谱柱（150 mm×4.6 mm,5μm）,以乙腈-0.2%磷酸溶液为流动相梯度洗脱,流速1.0 ml·min^-1,检测波长为230 nm（芍药苷、橙皮苷、黄芩苷）和280 nm（大黄酚）,柱温:40℃。结果:芍药苷、橙皮苷、黄芩苷和大黄酚分别在进样量为0.003⁰.592μg（r=0.999 9）,0.063¹.264μg（r=1.000 0）,0.205⁴.094μg（r=1.000 0）,0.008⁰.164μg（r=1.000 0）时与峰面积积分值呈良好的线性关系;平均回收率分别为99.49%（RSD=0.85%）,99.74%（RSD=0.71%）,99.75%（RSD=0.47%）,99.08%（RSD=1.28%）。结论:本法简便、准确,可用于消石利胆胶囊中芍药苷、橙皮苷、黄芩苷和大黄酚的含量测定。     

高效液相色谱法测定近视康合剂中芍药苷的含量

目的测定近视康合剂中芍药苷的含量。方法采用高效液相色谱法测定。以乙腈-0.05%磷酸二氢钾溶液（30：70）为流动相,检测波长为230nm,柱温为50℃。结果芍药苷在0.300～3.000μg（r=0.9990）范围内呈良好线性关系,芍药苷的平均回收率为99.00%（RSD=2.77%,n=5）。结论方法简便,分离效果好,结果准确可靠,可以用于近视康合剂的质量控制。     

五淋散胶囊中栀子苷和芍药苷的HPLC含量测定

目的：建立五淋散胶囊中栀子苷和芍药苷的HPLC含量测定方法。方法：采用Diamonsil C18色谱柱（250 mm×4.6 mm,5 μm）,流动相为甲醇-水（20∶80）,流速为1.0 mL?min-1,检测波长为235 nm;柱温为30 ℃;进样量为20 μL。结果：栀子苷进样量在0.162～1.296 μg范围内线性关系良好(r=0.999 9),平均回收率为101.30%,RSD为0.54%（n=6）;芍药苷在0.160～1.280 μg范围内线性关系良好(r=0.999 9),平均回收率为99.75%,RSD为1.04%（n=6）。结论：本方法简便、准确、快速、灵敏度高、重现性好,可作为五淋散胶囊中栀子苷和芍药苷的定量控制质量标准。     

HPLC法测定安宫降压丸中芍药苷的含量

目的建立HPLC法测定安宫降压丸中芍药苷含量的方法。方法采用Agilent-ODS C18色谱柱,流动相：乙腈-水（14∶86）,流速：1.0 mL/min,检测波长：230 nm。结果芍药苷进样量在0.044 48~0.556 0μg范围内呈良好的线性关系（r=0.999 9）,平均回收率为99.0%,RSD=1.8%（n=6）。结论该方法简便、准确、重复性好,可用于安宫降压丸中芍药苷的含量测定。     

高效液相色谱法测定红花逍遥片中4种有效成分的含量

目的建立同时测定红花逍遥片中芍药苷、芍药内酯苷、羟基红花黄色素A和甘草酸含量的高效液相色谱法。方法采用SHIMADZU LC 20AD高效液相色谱仪,Welch（ΜLtimate XB-C18,4.6mm×250 mm,5μm）色谱柱,以乙腈（A）-0.1%磷酸水溶液（B）为流动相,梯度洗脱,流速为1.0mL·min^-1,检测波长为403 nm（0¹0 min,检测羟基红花黄色素A）、230 nm（10¹5 min,检测芍药苷和芍药内酯苷）、237 nm（30⁴5 min,检测甘草酸）,柱温为25℃。结果红花逍遥片处方中4个成分芍药苷、芍药内酯苷、羟基红花黄色素A和甘草酸浓度分别在0.0094⁰.1880 mg·mL^-1（r=0.9997）、0.0037⁰.0744 mg·mL^-1（r=0.9996）、0.000 27⁰.005 40 mg·mL^-1（r=0.9998）、0.0050⁰.1010 mg·mL^-1（r=1.000）与峰面积呈良好的线性关系;平均回收率（n=6）分别为98.7%、98.2%、100.7%、100.8%。结论该方法准确可靠、重复性好,可用于红花逍遥片处方的质量控制。     

HPLC法同时测定固肾安胎丸中7种成分含量

摘要：目的:建立HPLC梯度洗脱法同时测定固肾安胎丸中2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、芍药内酯苷、芍药苷、苯甲酰芍药苷、川续断皂苷Ⅵ、续断苷A和续断苷B含量。方法:采用Diamonsil C18色谱柱（250 mm×4.6 mm,5μm）,流动相为乙腈-0.1%磷酸水溶液,梯度洗脱,流速为1.0 ml·min-1,柱温为25℃,检测波长分别为320 nm（2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷）、230 nm（芍药内酯苷、芍药苷、苯甲酰芍药苷）和212 nm（川续断皂苷Ⅵ、续断苷A和续断苷B）。结果:2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、芍药内酯苷、芍药苷、苯甲酰芍药苷、川续断皂苷Ⅵ、续断苷A和续断苷B质量浓度分别在2.98～74.50,5.66～141.50,9.88～247.00,0.89～22.25,10.77～269.25,1.99～49.75,1.06～26.50μg·ml-1范围内线性关系良好（r≥0.999 3）,平均加样回收率分别为97.77%,98.03%,99.22%,98.49%,100.03%,97.86%,96.89%,RSD分别为1.51%,1.11%,0.86%,1.18%,0.67%,1.29%,1.08%（n=9）。结论:该方法操作简便、重复性好,可用于固肾安胎丸中多指标性成分的质量控制。     

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.