HPLC测定龙胆泻肝丸中黄芩苷的含量

目的用高效液相色谱法测定龙胆泻肝丸中黄芩苷的含量.方法采用C18柱,以甲醇-水-冰醋酸(50∶50∶1)为流动相,检测波长为279nm测定.结果对照品在1.60～7.60μg/ml内呈线性关系,r=0.9998,加样回收率平均为99.0%,RSD为2.2%.结论本法准确、稳定、重复性好,可用于测定龙胆泻肝丸中黄芩苷的含量.     

高效液相色谱法测定龙胆泻肝丸中栀子苷的含量

目的:用高效液相色谱法测定龙胆泻肝丸中栀子苷的含量.方法:采用Thermo C18柱(4.6 mm×250 mm,5μm),以乙腈-水(15:85)为流动相,流速1.0 ml/min,检测波长为238 nm.结果:对照品在5.5～16.5μg/ml范围内呈线性关系,γ=0.999 8,加样回收率平均为97.2%(n=6),RSD为2.3%,结论:本方法简便、准确、重复性好,可用于测定龙胆泻肝丸中栀子苷的含量.     

龙胆泻肝丸中龙胆苦苷含量的检测方法

目的建立龙胆泻肝丸中龙胆苦苷含量测定的方法。方法色谱柱:VP-ODS柱(150mm×4.6mm,5μm);流动相:A组分:乙腈:0.1%磷酸溶液(10∶90);检测波长270nm;流速:1.0mL/min;柱温:25℃。结果龙胆苦苷的线性范围是0.3554～5.331μg,r=0.9998,平均回收率是100.04%,RSD=1.80%。结论该法可同时测定龙胆泻肝丸中龙胆苦苷和栀子苷的含量。     

HPLC测定龙胆泻肝丸中黄芩苷的含量

目的　用高效液相色谱法测定龙胆泻肝丸中黄芩苷的含量。方法　采用C18柱 ,以甲醇 水 冰醋酸 (5 0 ∶5 0 ∶1)为流动相 ,检测波长为 2 79nm测定。结果　对照品在 1.6 0～ 7.6 0 μg/ml内呈线性关系 ,r=0 .9998,加样回收率平均为 99.0 % ,RSD为2 .2 %。结论　本法准确、稳定、重复性好 ,可用于测定龙胆泻肝丸中黄芩苷的含量     

龙胆泻肝丸的质量标准补充研究

目的:对龙胆泻肝丸(水丸)质量标准进行补充研究。方法:采用薄层色谱法,对当归、泽泻、黄芩、柴胡、甘草、23-乙酰泽泻醇B、龙胆苦苷、栀子苷、甘草苷进行鉴别;采用HPLC法测定23-乙酰泽泻醇B的含量,色谱柱为Waters Symmetry C18(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸水溶液(62∶38),流速1.0 m L·min-1,柱温35℃,检测波长208 nm。结果:薄层色谱斑点清晰,分离度好,专属性强,重复性良好。23-乙酰泽泻醇B在20~2 000 ng范围内线性关系良好(r=0.999 9);平均回收率(n=6)为104.2%,RSD为0.9%。结论:本文建立的鉴别和含量测定方法可为龙胆泻肝丸(水丸)的质量标准完善提供参考。     

HPLC法测定龙胆泻肝丸中龙胆苦苷的含量

目的:建立以高效液相色谱(HPLC)法测定龙胆泻肝丸中龙胆苦苷含量的方法。方法:色谱柱为VP-ODS(150mm×4.6mm,5μm),流动相为乙腈-0.1%磷酸溶液(15∶85),检测波长为270nm,流速为1.0mL·min-1,柱温为25℃。结果:龙胆苦苷进样量在0.3554～5.331μg范围内与峰面积积分值呈良好线性关系(r=0.9998);平均回收率为100.05%,RSD=2.2%(n=6)。结论:本方法简便、快速、准确,可用于龙胆泻肝丸的质量控制。     

HPLC同时测定龙胆泻肝丸(浓缩丸)中龙胆苦苷、栀子苷和黄芩苷的含量

目的:建立同时测定龙胆泻肝丸(浓缩丸)中龙胆苦苷、栀子苷和黄芩苷的高效液相色谱分析方法.方法:采用安捷伦C 18(4.6mm×250mm,5μm)色谱柱,以甲醇(A)-0.2％磷酸溶液(B)为流动相,梯度洗脱(0～25min,20％A;25～30min,20％A→43％A;30～50min,43％A),流速:1.0mL/min,检测波长分别为280nm(黄芩苷、龙胆苦苷)和238nm(栀子苷);柱温:30℃.结果:龙胆苦苷在0.31754～3.1754μg之间线性关系良好,r=0.9996,栀子苷在0.16760～1.6760μg之间线性关系良好,r=0.9995,黄芩苷在0.16836～1.6836μg之间线性关系良好,r=0.9996,龙胆苦苷的平均回收率为98.63％,RSD=0.83％,栀子苷的平均回收率为97.98％,RSD=0.94％,黄芩苷的平均回收率为97.90％,RSD=1.02％.结论:该方法操作简单,重复性好,准确度高,分离效果好,可以用于龙胆泻肝丸(浓缩丸)的质量控制.     

HPLC测定龙胆泻肝丸中黄芩苷的含量

目的 用高效液相色谱法测定龙胆泻肝丸中黄芩苷的含量。方法 采用C18柱，以甲醇-水-冰醋酸(50：50：1)为流动相，检测波长为279nm测定。结果 对照品在1．60～7．60μg／ml内呈线性关系，r=0．9998，加样回收率平均为99．0％，RSD为2．2％．结论 本法准确、稳定、重复性好，可用于测定龙胆泻肝丸中黄芩苷的含量．     

HPLC法测定青果丸中黄芩苷的含量

目的:建立测定青果丸中黄芩苷含量的方法。方法:采用高效液相色谱法。色谱柱为Agilent TC-C18(150 mm×4.60mm,5μm),流动相为甲醇-水-0.02 mol/l磷酸(45∶55∶0.2,V/V/V),流速为1.0 ml/min,柱温为30℃,进样量为10μl,检测波长为278 nm。结果:黄芩苷检测质量浓度在10²00μg/ml范围内与峰面积积分值呈良好的线性关系(r=0.999 9,n=6);精密度、稳定性、重复性试验的RSD≤0.96%;平均加样回收率为99.53%,RSD=1.07%(n=9)。结论:该方法简便、准确、重复性好,可用于青果丸中黄芩苷的含量测定。     

基于指纹图谱和多成分含量测定的龙胆泻肝丸(水丸)质量研究

目的：建立龙胆泻肝丸(水丸)的HPLC指纹图谱,同时测定龙胆泻肝丸(水丸)中7个成分(栀子苷、龙胆苦苷、黄芩苷、汉黄芩苷、黄芩素、甘草酸、汉黄芩素)的含量,并基于指纹图谱和多成分含量测定结果评价产品质量。方法：采用CAPCELL PAK C₁₈(4.6 mm×250 mm,5 μm)色谱柱,以乙腈 -0.2%磷酸溶液为流动相进行梯度洗脱,流速1.0 mL·min^-1,检测波长254 nm,柱温25 ℃。建立龙胆泻肝丸(水丸)指纹图谱并进行相似度分析,同时测定其中7个成分含量。结果：在指纹图谱研究中,以黄芩苷为参照峰,共标定20个共有峰,并指认出7个色谱峰,采用指纹图谱相似度评价系统(2012年版) 进行相似度分析,30批龙胆泻肝丸(水丸)相似度在0.815~1.000。7个化学成分线性关系良好,加样回收在97.7%~104.3%之间,RSD均小于2.0%。30批样品中栀子苷、龙胆苦苷、黄芩苷、汉黄芩苷、黄芩素、甘草酸、汉黄芩素的质量分数依次为2.48~3.59、1.90~6.11、3.51~8.09、0.59~1.70、0.18~1.95、 0.90~1.63、0.10~0.87 mg·g^-1。结论：研究建立的HPLC指纹图谱结合多成分同时测定的方法,操作简便,结果准确、稳定,可为龙胆泻肝丸(水丸)的质量评价提供参考。     

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.