高效液相色谱法测定冬凌草糖浆中冬凌草甲素含量

目的 建立测定冬凌草糖浆的冬凌草甲素含量的高效液相色谱法.方法采用Diamonsil C18色谱柱(250mm×4.6mm,5μm),以甲醇-水(50:50)为流动相,流速为1.0 mL/min,检测波长为239 nm.结果冬凌草甲素进样量在0.093～0.746μg范围内与峰面积积分值线性关系良好,回归方程为Y=413 933.35-63 428.66X,r=0.999 7(n=5);平均加样回收率为99.0%,RSD为1.06%(n=5).结论该法简便、准确、专属性和重复性好,为冬凌草糖浆中冬凌草甲素的定量分析提供了科学有效的方法.     

半夏糖浆质量标准研究

目的研究半夏糖浆（麻黄、枇杷叶、陈皮等）内在质量的控制方法。方法采用薄层色谱（TLC）法对方中的枇杷叶、陈皮、甘草3味药材进行定性鉴别；用高效液相色谱（HPLC）法对方中麻黄的有效成分盐酸麻黄碱进行含量测定。结果定性鉴别薄层色谱特征明显，专属性强；方法学考察表明，盐酸麻黄碱进样量在0．0854-0．5126μg范围内与峰面积具有良好的线性关系（r=0.9999），平均回收率为99．30％（n=9），RSD=0.31％。结论方法准确、可靠、重现性好，可用于半夏糖浆的质量控制。     

复方丹参软胶囊质量标准的研究

目的：改进复方丹参软胶囊质量标准。方法：采用TLC鉴别处方中丹参、三七；采用RP－HPLC法测定复方丹参软胶囊中丹参酮ⅡA的含量，色谱条件：Diamonsil C18柱；流动相：甲醇－水（73：27）；流速：1.5ml/min；检测波长：270nm。结果：含量测定线性范围8－80μg/ml,r=0.9999。加样回收率99.60%,RSD=1.10%。结论：建立了专属性较强的薄层色谱鉴别并解决了辅料（PEG）对薄层展开的干扰；采用高效液相色谱法测定复方丹参软胶囊中丹参酮ⅡA的含量，方法简便，准确，灵敏度高，重现性好，其他组分对测定无干扰，可用于该制剂的质量控制。     

UPLC法同时测定冬凌草中5种有效成分的含量

目的:建立超高效液相色谱法同时测定冬凌草药材中冬凌草甲素、冬凌草乙素、迷迭香酸、齐墩果酸和熊果酸5个主要有效成分的含量。方法:采用WATERS UPLC色谱系统,ACQUITY BEH Shield RP18色谱柱(2.1 mm×100 mm,1.7μm);流动相为0.1%甲酸甲醇溶液(A)-0.1%甲酸水溶液(B),梯度洗脱(0～9 min,70%A→57%A;9～10 min,57%A→48%A;10～11 min,48%A→48%A;11～14 min,48%A→14%A;14～22 min,14%A→14%A),流速0.2 mL·min-1;检测波长为250 nm(0～12.40min测定冬凌草甲素、冬凌草乙素和迷迭香酸)和210 nm(12.41～22.00 min测定齐墩果酸和熊果酸);柱温23℃。结果:本方法可在22 min内完成5个成分的色谱分析,且各成分色谱峰之间具有良好的分离度;冬凌草甲素、冬凌草乙素、迷迭香酸、齐墩果酸和熊果酸的线性范围分别为0.110～0.990μg(r=0.9997),0.012～0.108μg(r=0.9991),0.030～0.270μg(r=0.9993),0....     

不同产地冬凌草定性定量质量评价

目的建立冬凌草药材的定性定量研究方法,并评价不同产地冬凌草的质量。方法采用薄层色谱法对冬凌草中齐墩果酸和冬凌草甲素进行定性鉴别,高效液相色谱法测定冬凌草甲素含量。结果齐墩果酸和冬凌草甲素的薄层鉴别图谱斑点清晰,冬凌草甲素在3.100 8～31.008μg与峰面积线性关系良好,r=0.999 9,平均含量为0.35%,回收率为99.7%,RSD为1.3%。结论本法简便、准确、灵敏度高、重复性好,可以保证冬凌草药材质量可控。     

川贝清肺糖浆质量标准研究

目的建立川贝清肺糖浆的质量标准。方法采用薄层色谱(TLC)法对方中枇杷叶、甘草进行薄层色谱鉴别,对苦杏仁进行理化鉴别。采用反相高效液相色谱法测定甘草酸含量,色谱柱为Discovery C18柱(150 mm×4.6 mm,5μm),乙腈-水-冰醋酸(35∶65∶2)为流动相,流速为1 mL/min,柱温为27℃,检测波长为250 nm。结果薄层色谱中,供试品溶液在与对照药材溶液色谱相应位置上显相同颜色的斑点。甘草酸进样质量浓度0~224μg/mL范围内与峰面积呈线性良好关系(r=0.999 9,n=6),平均加样回收率为98.92%,RSD=1.03%(n=6)。结论该法简便、准确、可靠、专属性强、重现性好,可作为川贝清肺糖浆的质量标准。     

HPLC法测定小儿白贝止咳糖浆中原阿片碱的含量

目的：建立小儿白贝止咳糖浆中原阿片碱的含量测定方法。方法：采用高效液相色谱法测定，色谱条件为：Agilent TC C18 色谱柱(250mm×4.6 mm，5 μm)，流动相为乙腈-三乙胺醋酸溶液（18 : 82），流速1 mL? min-1，检测波长289 nm，柱温30 ℃。结果：原阿片碱在0.1395～2.2323 μg范围内线性关系良好（r = 0.999 8），平均回收率99.14 %（RSD=0.82 %）。3批样品含量测定结果：平均含量为6.6 μg?mL-1。结论：本方法简便、准确、重现性好，可以作为小儿白贝止咳糖浆的控制方法。     

祛风止痛胶囊质量标准研究

目的：对祛风止痛胶囊的质量标准进行提高。方法：用薄层色谱法对祛风止痛胶囊中续断、威灵仙进行定性鉴别；用HPLC法测定川续断皂苷Ⅵ的含量，采用Appllo C18柱（4.6mm×250mm，5μm）,流动相为乙腈-水（30∶70）,流量1.0mL?min-1,柱温30℃,检测波长为212nm。结果：薄层色谱鉴别方法斑点清晰，重现性好；川续断皂苷Ⅵ在0.87～11.72μg范围内线性关系良好（r=1.0000）,加样回收率为96.0%,其RSD为1.4%（n=6）。结论：所建方法可靠、准确，可用于该制剂的质量控制。     

补康灵糖浆质量标准研究

目的建立补康灵糖浆的质量标准。方法采用薄层色谱法对补康灵糖浆中丹参、茯苓进行鉴别,采用高效液相色谱法对补康灵糖浆中黄芪甲苷进行含量测定。结果薄层色谱图斑点清晰,阴性对照无干扰。黄芪甲苷平均回收率为99．25％,RSD=0．88％（n=9）。结论该方法简便、准确、重现性好,能有效控制补康灵糖浆的质量。     

牛黄化毒片的质量标准研究

目的：建立牛黄化毒片的质量标准。方法：采用薄层色谱法对该制剂中的连翘、甘草和人工牛黄进行鉴别,采用高效液相色谱法测定制剂中欧前胡素的含量。色谱柱：Agilent zorbax SB-C18色谱柱（4.6 mm×250 mm,5μm）;流动相：乙腈-水（52∶48）;流速：1.0 ml/min;柱温30℃;检测波长为300 nm。结果：薄层色谱斑点清晰,重现性好;欧前胡素的平均加样回收率为98.77%,RSD为0.67%（n=6）。结论：该方法准确可靠,重复性好,为牛黄化毒片的质量控制和评价提供了依据。     

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.