HPLC测定薄膜衣片剂中食用色淀的含量

目的 建立薄膜衣片剂中食用色淀的HPLC含量测定新方法.方法 高效液相色谱梯度洗脱法.色谱柱:Alltima-C18 (4.6 mm×250 mm,5 μm);流动相:甲醇(A)-0.05 mol·L-1醋酸铵水溶液(B)梯度洗脱;检测波长:254 nm;流速:1.0 mL· min-1;进样量为20 μL.结果 柠檬黄色素和日落黄色素分别在10.03～200.6 μg·mL-1和10.01～200.2 μg·mL-1范围内呈良好线性关系(r≥0.999 9),色淀总的平均回收率为96.7%,RSD=1.26%.结论 所建立的方法操作简便、灵敏度高、重复性好,为薄膜衣片剂中食用色淀含量提供有效的质量控制,建立了新的检测方法.     

高效液相色谱法测定药用辅料日落黄的含量

目的 建立高效液相色谱法测定药用辅料日落黄的含量.方法 采用安捷伦C18柱(4.6 mm×250 mm,5 μm),以甲醇-0.02 mol·L-1乙酸铵溶液(30∶70)为流动相,流速为1.0 mL· min-1,检测波长为236 nm,柱温为35℃.结果 日落黄线性范围为5.55～111.03 μg·mL-1,r=0.999 9,平均回收率为100.0％,RSD=0.23％.结论 改进后的方法简单、准确,能控制本品的质量.     

高效液相色谱法测定护肝宁片中大黄素的含量

目的 建立HPLC法测定护肝宁片中大黄素的含量.方法 色谱柱C18柱(4.6 mm× 250 mm);流动相:甲醇-0.1%磷酸(85:15);流速:1.0 ml·min-1;检测波长:254 nm;柱温: 30 ℃,进样量:10 μL.结果 在3.86 μg·mL-1～19.30 μg·mL-1浓度范围内与峰面积呈良好的线性关系.回归方程Y=34295061.35X 1941.0407,(r=0.9998)平均回收率为99.4%(n=9).结论 本法简便快速,定量准确,可用于护肝宁片的质量控制.     

琥乙红霉素片含量测定方法的改进

目的:改进琥乙红霉素片剂含量的测定方法.方法:采用高效液相色谱法,以Waters XBridgeTM Shied C18(250 mm×4.6 mm,5 μm)为色谱柱;0.067 mol·L-1磷酸二氢铵溶液(用三乙胺调节pH至6.5)-乙睛(65:35)为流动相;检测波长210 nm;流速为1.0 ml·min-1;柱温为20℃.结果:红霉素A在39.83～139.41 μg·ml-1范围内呈良好的线性关系(r=0.999 3),平均回收率为98.6%(RSD=0.9%,n=9),检测限为1.19 μg,定量限为3.58 μg.将该法测定结果与效价法测定的含量进行比较,结果基本一致.结论:该方法更简便、准确,重复性好.     

高效液相色谱法测定酮洛芬凝胶的含量

目的建立HPLC法测定酮洛芬凝胶剂的含量,为质量控制提供有效的分析手段.方法色谱柱为Dikma Technologies DiamonsilTM C18(4.6 mm×250 mm,5 μm);流动相为甲醇-0.05mol·L-1 磷酸二氢钾溶液(73);流速为1.0 mL·min-1;柱温为35℃;检测波长为255 nm.结果制剂中辅料和有关物质对主药无干扰,酮洛芬在1.0～18.0 mg·L-1,r=0.999 7(n=5)范围内呈良好线性关系;平均回收率分别为100.1%(RSD=1.18%),100.68%(RSD=1.24%),99.0%(RSD=0.43%).结论该法操作简便,结果准确、专属性强,可有效控制本品质量.     

HPLC法同时测定康复新液中尿嘧啶、次黄嘌呤及肌苷含量

目的:建立HPLC法同时测定康复新液中的尿嘧啶、次黄嘌呤及肌苷含量.方法:色谱柱:Wates SunfireTM C18柱(250 mm×4.6 mm,5 μm );甲醇-3%甲醇溶液(含0.07%醋酸)梯度洗脱;检测波长254 nm;进样量:10 μl.结果:尿嘧啶在4.92～34.44 μg·ml-1 (r=0.999 9),次黄嘌呤在12.43～87.06 μg·ml-1(r=0.999 9),肌苷在24.77～173.40μg·ml-1(r=0.999 9)的浓度范围内呈良好的线性关系.尿嘧啶的平均回收率为102.63%(RSD=1.78%);次黄嘌呤的平均回收率为99.13%(RSD=1.89%);肌苷的平均回收率为98.98%(RSD=1.33%).结论:该法操作简便、准确,重复性、稳定性好,可用于同时检测康复新液中尿嘧啶、次黄嘌呤及肌苷的含量.     

HPLC法测定复方鱼腥草合剂中绿原酸、黄芩苷的含量

目的:建立同时测定复方鱼腥草合剂中绿原酸、黄芩苷的高效液相色谱法.方法:采用Sinochrom ODS-BP(250 mm×4.6 mm,5 μm)色谱柱;流动相为甲醇:0.2%磷酸溶液,进行梯度洗脱;柱温:30℃流速为0.9 ml·min-1,检测波长为315 nm.结果:绿原酸在0.1～1.0 μg·ml-1范围内线性关系良好(r=0.999 5),平均回收率为100.26%,RSD=0.53%(n=9);黄芩苷在1.8～18.0 μg·ml-1范围内线性关系良好(r=0.996 6),平均回收率为100.04%,RSD=0.87%(n=9).结论:本方法简便易行,能够准确、快速测定复方鱼腥草合剂中的绿原酸和黄芩苷的含量.     

RP-HPLO法测定甲硝唑栓的含量

目的 建立高效液相色谱法来检测甲硝唑栓的含量.方法 采用色谱柱:Thermo C18(250mm×4.6mm,5μm);流动相:甲醇-50 mm01·L-1磷酸二氢钾溶液(20:80),流速:1.0ml·min-1;柱温30℃;检测波长:310nm;进样量:20 μ1.结果 本研究建立的检测方法能在该色谱条件下把甲硝唑与其辅料完全分离开来,回归方程分别为:A=3.47 X 104C-0.88 X 104,r=0.9999(n=3),回收率为98.4%,RSD为0.9%.结论 该检测技术具有快速、简便、灵敏、重复性好、便于操作、专属性强等优点.     

双波长HPLC法同时测定止痢宁片中穿心莲内酯和脱水穿心莲内酯的含量

目的:建立高效液相色谱法同时测定止痢宁片中穿心莲内酯和脱水穿心莲内酯含量的方法.方法:色谱柱:CAPCELL PAK-C18柱(150 mm×4.6 mm,5 μm);流动相:甲醇-水(48:52);流速为1.0 ml·min-1;柱温:30℃;检测波长:225 nm(穿心莲内酯)、250 nm(脱水穿心莲内酯);进样量:5 μl.结果:穿心莲内酯在4.17～41.68 μg·ml-1 (r=0.999 9)、脱水穿心莲内酯在4.04～40.40 μg·ml-1(r=0.999 9)浓度范围内线性关系良好;穿心莲内酯回收率为99.21%(RSD=1.3%,n=6),脱水穿心莲内酯回收率98.73%(RSD=1.1%,n=6).结论:该方法简单、准确,可作为止痢宁片的质量控制.     

HPLC法同时测定复方槐花口服液中柚皮苷和黄芩苷的含量

目的:建立HPLC法同时测定复方槐花口服液中柚皮苷、黄芩苷的含量.方法:色谱柱:Agilent ZORBAX SB- C18(250 mm×4.6 mm,5 μm);流动相:乙腈-0.1%磷酸溶液(23:77);检测波长:280 nm;流速:1.0 ml·min-1;柱温:30℃.结果:柚皮苷和黄芩苷分别在0.194～1.742 μg·ml-1(r=0.999 5,n=5)和0.419～3.773 μg·ml-1(r=0.999 8,n=5)范围内与峰面积呈良好线性关系,平均加样回收率为100.06%,RSD为1.10%(n=6)和99.27%,RSD为1.43%(n=6).结论:HPLC法操作简便,结果准确,可用于复方槐花口服液的质量控制.     

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.