HPLC法测定苦参总碱中苦参碱与氧化苦参碱的含量

目的:采用高效液相色谱法测定苦参总碱中苦参碱和氧化苦参碱的含量。方法:采用 Elite Hypersil NH_2柱(5μm,250mm×4.6 mm),乙腈-无水乙醇-3%磷酸溶液(81:10:9)为流动相,流速:1.0 mL·min~(-1),检测波长220 nm,柱温:25℃,进样量:10 μL。结果:苦参碱、氧化苦参碱的线性范围分别为5.32～53.2μg·mL~(-1)(r=0.9997),65.7～525.6μg·mL~(-1)(r=0.9995)。苦参碱平均加样回收率为99.5%,RSD=1.0%(n=6);氧化苦参碱的平均加样回收率为99.7%,RSD=0.6%(n=6)。结论:本方法操作简便、快速、可靠,可用于控制苦参总碱质量。     

HPLC法测定复方对乙酰氨基酚片中对乙酰氨基酚、乙酰水杨酸及咖啡因的含量

目的:采用高效液相色谱法测定复方对乙酰氨基酚片中对乙酰氨基酚、乙酰水杨酸及咖啡因的含量。方法:采用 Li-chrospher C_(18)(5 μm,4.6 mm×250 mm)色谱柱,以甲醇-水-冰醋酸(40:60:0.3)为流动相,流速1.0 mL·min~(-1),检测波长272 nm,柱温35℃。结果:对乙酰氨基酚线性范围为19.93～199.32μg·mL~(-1)(r=0.9998),平均回收率(n=9)为99.2%;乙酰水杨酸线性范围为36.00～359.96μg·mL~(-1)(r=0.9999),平均同收率(n=9)为99.7%;咖啡因线性范围为4.90～49.04μg·mL~(-1)(r=0.9998),平均同收率(n=9)为98.8%。结论:方法简使,结果准确,适用于该产品的质量控制。     

RP-HPLC法测定痹痛宁胶囊中士的宁和马钱子碱的含量

采用反相高效液相色谱法测定痹痛宁胶囊中士的宁和马钱子碱的含量。色谱柱CAP-CELL C18(4.6 mm×150 mm,5μm);流动相:水-乙腈(80∶20)(含三乙胺0.01 mol·L-1,用磷酸调pH至2.6±0.1);检测波长260 nm;流速1.0 mL·min-1;柱温25℃。测得士的宁和马钱子碱的浓度分别为0.2097～3.1455μg(r=0.9996)和0.0952～1.4280μg(r=0.9994),平均回收率(n=9)分别为99.2%、99.3%。     

HPLC法测定板蓝根药材中靛蓝和靛玉红的含量

目的:采用 HPLC—UV 法测定板蓝根中靛蓝和靛玉红含量。方法:将板蓝根经氯仿回流提取,然后用 HPLC 测定。色谱柱为 Diamonsil~(TM)C_(18)(250 mm×4.6 mm,5μm),流动相为乙腈-0.05%磷酸梯度洗脱,流速为1.0 mL·min~(-1),检测波长为300 nm,柱温为30℃。结果:靛蓝线性范围为0.1488～9.520μg·mL~(-1)(r=0.9999,n=7),平均回收率为97.8%,RSD=1.7%(n=6);靛玉红线性范围为0.2539～16.25μg·mL~(-1)(r=0.9995,n=7),平均回收率为98.5%,RSD=1.64%(n=6)。结论:所用方法准确可靠,适合于板蓝根药材的质量控制。     

HPLC法同时测定芩连片中黄芩苷和小檗碱的含量

目的:建立 HPLC 法同时测定芩连片中黄芩苷和小檗碱含量。方法:以芩连片为研究对象,采用 Kromasil ODS(200 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-0.05 mol·L~(-1)磷酸二氢钾溶液-三乙胺(26:74:0.2),流速1.0 mL·min~(-1),检测波长277 nm,柱温为室温。结果:黄芩苷、小檗碱分别在0.0101～0.1217 mg·mL~(-1)(r=0.9997,n=7),0.0114～0.1372 mg·mL~(-1)(r=0.9998,n=7)范围内呈良好线性关系;平均回收率(n=9)分别为98.7%和97.7%。结论:本测定方法简便、快速、准确,为芩连片质量评价提供了依据。     

HPLC法同时测定泌感颗粒中小檗碱和槲皮素的含量

目的:建立同时测定泌感颗粒中小檗碱和槲皮素含量的方法。方法:采用高效液相色谱法,色谱柱为 Diamonsil C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.05 mol·L~(-1)磷酸二氢钾溶液(27:73),流速为1.0 mL·min~(-1),检测波长为360nm。结果:小檗碱浓度在8.33～41.6μg·mL~(-1)范围内线性关系良好(r=0.9997),平均方法回收率(n=6)为98.6%;槲皮素浓度在4.08～20.4μg·mL~(-1)范围内线性关系良好(r=0.9998),平均方法回收率(n=6)为97.8%;结论:本法简便,准确度和重复性好,可用于泌感颗粒中小檗碱和槲皮素的同时测定。     

RP-HPLC—ECD测定通脉颗粒中3种化合物

目的:建立测定通脉颗粒中原儿茶醛、阿魏酸和黄芩苷的 RP-HPLC-ECD 分析方法。方法:采用 RP-HPLC-ECD 检测法,以 Zorbax SB—C_(18)(150 mm×4.6 mm,5.0 μm)为色谱柱,甲醇(A)、2%醋酸(B)为流动相,梯度洗脱,流速为1.0 mL·min~(-1);电化学检测器的工作电位为0.9 V;柱温为30℃。结果:原儿茶醛、阿魏酸和黄芩苷的线性范围分别为0.138～12.4μg·mL~(-1)(r=0.9999),0.130～11.7μg·mL~(-1)(r=0.9992)和0.192～240μg·mL~(-1)(r=0.9998);平均加样回收率(n=6)分别为97.4%(RSD=0.8%),98.7%(RSD=2.3%)和97.9%(RSD=2.9%)。结论:该法快速、灵敏、准确,可为通脉颗粒的质量控制提供科学依据。     

HPLC法测定止痛风湿丸中马钱子碱和士的宁的含量

目的建立止痛风湿丸中马钱子碱和士的宁的高效液相色谱的分析法。方法采用lunaC18色谱柱(4.6mm×250mm,5μm);流动相为乙腈-0.01mol/L庚烷磺酸钠与0.02 mol/L磷酸二氢钾等量混合液(用10%磷酸调节pH值至2.8)(22∶78);流速1.0mL/min;检测波长为260nm。结果马钱子碱在0.06608～1.652μg(r=0.99988)、士的宁在0.04064～1.0160μg(r=0.99998),范围内呈良好的线性关系;马钱子碱平均回收率为98.4%,RSD为1.1%;士的宁平均回收率为98.6%,RSD为1.0%。结论本方法准确可靠,简便灵敏,重现性好,可用于止痛风湿丸中马钱子碱和士的宁的质量控制。     

RP-HPLC法同时测定祛风活络丸中士的宁和马钱子碱的含量

目的:建立祛风活络丸中士的宁和马钱子碱的反相高效液相分析法,为该药质量控制提供依据.方法:采用Techsphese-C18ODS色谱柱(4.6 mm×250mm,5μm);乙腈-甲醇-0.05 mol·L-1KH2PO4溶液-三乙胺(25:19:55:1,磷酸调pH至3.5)为流动相:流速1 mL·min-1;检测波长254 nm.结果:士的宁在0.3～3.6μg(r=0.999 9)、马钱子碱在0.2～2.4μg(r=0.999 6)范围内呈良好的线性关系:士的宁回收率为97.6%,RSD=2.0%;马钱子碱回收率为101.02%,RSD=1.4%.结论:本方法准确可靠,简便灵敏,重现性好,可用于祛风活络丸中士的宁和马钱子碱的质量控制.     

HPLC法同时测定天山雪莲中紫丁香苷、绿原酸和芦丁的含量

目的:采用液相色谱法同时测定天山雪莲中紫丁香苷、绿原酸和芦丁的含量。方法:Kromasil ODS-1色谱柱(250 mm×4.6 mm,5μm),柱温为35℃;以乙腈(A)-0.4%磷酸(B)为流动相,梯度洗脱(0 min,13%A;15 min,13%A;16 min,15%A;40 min11,15%A),流速1 mL·min~(-1);双波长检测:257 nm(检测紫丁香苷、芦丁),327 nm(检测绿原酸)。结果:紫丁香苷存5.104～51.04 μg·mL~(-1)(r=0.9998)、绿原酸在38.82～258.8μg·mL~(-1)(r=0.9991)、芦丁在39.42～262.8μg·mL~(-1)(r=0.9997)范围内都呈良好线性关系;紫丁香苷、绿原酸和芦丁的回收率分别为99.7%(RSD=1.0%),102.9%(RSD=1.5%),101.7%(RSD=1.2%);供试品溶液在12 h 内稳定。结论:该方法快速简单,线性关系良好。     

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.