RP—HPLC法同时测定白芍中芍药苷和芍药内酯苷的含量

目的:建立了RP-HPLC法对白芍中芍药苷和芍药内酯苷同时定量,考察不同产地白芍中芍药苷、芍药内酯苷的含量。方法:高效液相色谱法,Hypersil-C_(18)色谱柱(4.6 mm×200 mm,5 μm),流动相:甲醇-乙腈-水(10:10:80),流速0.8 mL·min~(-1),检测波长230nm,柱温为室温。以咖啡因为内标测定了白芍中芍药苷和芍药内酯苷的含量。结果:芍药苷、芍药内酯苷浓度与峰面积呈良好的线性关系,线性范围分别是:芍药苷18.24～273.6μg·mL~(-1),r=0.999 6(n=7);芍药内酯苷4.96～74.4μg·mL~(-1),r=0.999 7(n=7);回收率(n=9)芍药苷为97.5％～97.7％,芍药内酯苷为91.1％～96.3％。结论:本方法测定了26个不同产地、不同批号及炮制品的白芍样品中芍药苷、芍药内酯苷含量,该方法分离度好,快速,简便,重现性好。     

HPLC法测定乳痛丸中芍药苷和阿魏酸的含量

目的 建立HPLC法同时测定乳痛丸中芍药苷、阿魏酸含量的方法.方法 Agilent-ODS C18色谱柱;流动相:乙腈-0.10％磷酸水溶液(14∶86);流速:1 mL·min-1;检测波长:230 nm;柱温:35℃.结果 芍药苷选样量在0.03086～0.3086 μg范围内线性关系良好(r=0.9994),平均回收率为98.56％ (RSD=1.33％);阿魏酸在0.01548～0.1548 μg范围内线性关系良好(r=0.9996),平均回收率为98.11％ (RSD=1.18％).结论 本法操作简便、结果准确,可用于同时测定乳痛丸中芍药苷、阿魏酸的含量.     

HPLC法测定麻仁润肠丸中芍药苷的含量

目的:建立HPLC法测定麻仁润肠丸中芍药苷的含量.方法:色谱柱:Agilent Zorbax SB-C18(150 mm×4.6 mm,5μm);流动相:甲醇-水(25∶75);流速:1.0 ml·min-1;检测波长:230 nm;柱温:室温;进样量:10μl.结果:芍药苷进样量在0.012 ～0.232 g范围内与峰面积线性关系良好(r=0.999 9),平均回收率为100.35％,RSD为1.47％(n=6).结论:本方法操作快速、结果准确,可用于麻仁润肠丸中芍药苷的含量测定.     

高效液相色谱法测定白芍药材中芍药苷和芍药内酯苷的含量

目的:建立高效液相色谱法测定白芍药材中芍药苷和芍药内酯苷含量的方法.方法:采用高效液相色谱法,色谱柱:Kromasil ODS2 (4.6 mm×250 mm,5 μm),流动相:甲醇-0.1％磷酸溶液(用1％氢氧化钠溶液调节pH值至4.2)(34:66);流速:1.0 mL·min-1,检测波长:230 nm.结果:芍药内酯苷在0.018～0.576 μg范围内呈线性关系(r=0.9999),芍药苷在0.028～0.896μg范围内呈线性关系(r=0.9999);芍药内酯苷加样回收率为98.18％(n=6),RSD值小于2％,芍药苷加样回收率为98.26％(n=6),RSD值小于2％.结论:本研究所建方法灵敏、简便,能同时准确测定白芍药材中芍药苷和芍药内酯苷的含量.     

反相高效液相色谱法测定和络舒肝丸中芍药苷含量

目的建立测定和络舒肝丸中芍药苷含量的反相高效液相色谱法(RP-HPLC法)。方法采用Diamonsll C18柱(250 mm×4.6 mm, 5μm)为色谱柱,流动相为乙腈-0．2％磷酸溶液(18:82),流速为1．0 mL／min,检测波长为230 nm。结果芍药苷进样量在0．1～0.9μg范围内与峰面积线性关系良好,回归方程Y=1 180．28X+16．79(r=0．999 6),平均加样回收率为97．84％,RSD=1．27％(n=5)。结论RP-HPLC法操作简单,重现性好,可作为该丸剂中芍药苷的含量测定。     

HPLC测定芍药丸中芍药苷的含量

目的 建立HPLC测定芍药丸中芍药苷含量的方法.方法 采用色谱柱为:Inertsil ODS-3C18(250 mm×4.6 mm,5μm);流动相:甲醇-1%磷酸溶液(35:65);柱温:40 ℃;流速:1.0 ml/min;检测波长为230 nm.结果 芍药苷含量在4.92～49.2 μg/ml,线性关系良好(r=0.999),平均回收率98.64%.结论 该法快速、简便、准确,可用于芍药丸的质量控制.     

RP-HPLC法测定固经丸中芍药苷的含量

目的:建立HPLC法测定固经丸中芍药苷的含量。方法:ZORBAX SB-C_(18)分析柱(250 mm×4.6 mm,5μm);流动相:甲醇-0.05 mol·L~(-1)磷酸二氢钾溶液-三乙胺(28:72:0.5);检测波长:230 nm;流速:1.0 ml·min~(-1),柱温:40℃。结果:芍药苷在0.44～3.96μg范围内的线性关系良好(r=0.9999),平均加样回收率为99.2%(n=5),RSD 1.2%(n=5)。结论:该方法准确,灵敏度高,重现性好。     

HPLC法测定活血祛瘀止痛丸中芍药苷的含量

目的 采用高效液相色谱法建立活血祛瘀止痛丸中芍药苷的测定方法.方法 采用Thermo BDS Hypersil C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.1％磷酸溶液(15:85)为流动相,流速:1.0 mL·min-1,检测波长:230 nm.结果 芍药苷进样量在0.120 6～2.413μg之间与峰面积呈良好的线性关系(r=0.999 9),平均回收率为99.0％,RSD为0.9％(n=6).结论 该法简便快捷,结果准确可靠,可用于该制剂的质量控制.     

HPLC法测定乳痛丸中芍药苷的含量

目的 建立乳痛丸中芍药苷的含量测定方法.方法 采用Puritex C18色谱柱,甲醇-0.05 mol·L-1磷酸二氢钾溶液(37;63)为流动相,流速:0.6 mL·min-1,检测波长:230 nm,柱温:室温.结果 芍药苷在0.504～30.8 μg·mL-1浓度范围内线性关系良好(r=0.999 8,n=7).平均加样回收率为98.74％(n=9),RSD为1.09％.结论 本法简便、灵敏、结果准确,可用于乳痛丸质量控制中的含量测定.     

HPLC法测定舒胃丸中芍药苷含量

目的建立舒胃丸中芍药苷的高效液相色谱法含量测定方法。方法选用ODSC18色谱柱;以乙腈-水-磷酸(15∶85∶0.05)为流动相;检测波长:230nm;柱温:室温;流速:1.0mL·min-1。结果芍药苷在1.042～5.210μg范围内线性关系良好(r=0.9996),平均回收率为98.77%,RSD=1.28%(n=5)。结论本方法准确,简便,灵敏,可靠,可用于该制剂的质量控制。     

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.

     

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.     

2-(Acetoxyphenyl)-(Z)-styryl sulfides as cyclooxygenase inhibitors

2-(Acetoxyphenyl)-(Z)-styryl sulfides are described as selective cyclooxygenase-2 (COX-2) inhibitors, useful for treating inflammation and COX-2-mediated disorders including neoplasia. 2-(Acetoxyphenyl)-(Z)-styryl sulfide is claimed to be the most potent COX inhibitor in the series with a COX-2 selectivity ratio of 33. This compound is also claimed to be superior to celecoxib (Celebrex^®, Pfizer) in inhibiting cell growth of colorectal carcinoma cells. In this evaluation, the COX inhibitory activity of this compound is compared to that previously disclosed for diarylheterocycles and 2-(acetoxyphenyl)alkyl sulfides. The validity of the DLD-1 cell line in the growth inhibition studies is questioned based on recent literature reports indicating the lack of COX-2 expression in this cell line.     

Sleep-disordered breathing with chronic opioid use

Chronic opioid use for pain relief or as substitution therapy for illicit drug abuse is prevalent in our societies. In the US, retail distribution of methadone and oxycodone has increased by 824 and 660%, respectively, between 1997 and 2003. μ-Opioids depress respiration and deaths related to illicit and non illicit chronic opioid use are not uncommon. Since 2001 there has been an emerging literature that suggests that chronic opioid use is related to central sleep apnoea of both periodic and non-periodic breathing types, and occurs in ～ 30% of these subjects. The clinical significance of these sleep-related abnormalities are unknown. This review addresses the present knowledge of control of ventilation mechanisms during wakefulness and sleep, the effects of opioids on ventilatory control mechanisms, the sleep-disordered breathing found with chronic opioid use and a discussion regarding the future research directions in this area.     

Drug targets for cognitive enhancement in neuropsychiatric disorders

The investigation of novel drug targets for treating cognitive impairments associated with neurological and psychiatric disorders remains a primary focus of study in central nervous system (CNS) research. Many promising new therapies are progressing through preclinical and clinical development, and offer the potential of improved treatment options for neurodegenerative diseases such as Alzheimer's disease (AD) as well as other disorders that have not been particularly well treated to date like the cognitive impairments associated with schizophrenia (CIAS). Among targets under investigation, cholinergic receptors have received much attention with several nicotinic agonists (α7 and α4β2) actively in clinical trials for the treatment of AD, CIAS and attention deficit hyperactivity disorder (ADHD). Both glutamatergic and serotonergic (5-HT) agonists and antagonists have profound effects on neurotransmission and improve cognitive function in preclinical experiments with animals; some of these compounds are now in proof-of-concept studies in humans. Several histamine H3 receptor antagonists are in clinical development not only for cognitive enhancement, but also for the treatment of narcolepsy and cognitive deficits due to sleep deprivation because of their expression in brain sleep centers. Compounds that dampen inhibitory tone (e.g., GABA_A α5 inverse agonists) or elevate excitatory tone (e.g., glycine transporter inhibitors) offer novel approaches for treating diseases such as schizophrenia, AD and Down syndrome. In addition to cell surface receptors, intracellular drug targets such as the phosphodiesterases (PDEs) are known to impact signaling pathways that affect long-term memory formation and working memory. Overall, there is a genuine need to treat cognitive deficits associated with many neuropsychiatric conditions as well as an increasingly aging population.