HPLC法测定黄连上清片中4种成分的含量

摘 要 目的： 提高黄连上清片质量标准,建立同时测定绿原酸、栀子苷、黄芩苷、盐酸小檗碱4种成分含量的方法。方法: 采用高效液相色谱法,色谱柱为DiamonsilTM C₁₈(250 mm×4.6 mm,5 μm),流动相为二元梯度系统,其中溶剂A为乙腈,溶剂B为0.3%磷酸水溶液,流速为1.0 ml·min^-1,检测波长为238 nm,柱温30℃,进样量为10 μl。结果: 绿原酸、栀子苷、黄芩苷、盐酸小檗碱的线性范围分别为8.11～81.10 μg·ml^-1(r=0.999 7)、13.08～130.80 μg·ml^-1(r=0.999 7)、10.76～107.60 μg·ml^-1(r=0.999 8)、7.92～79.20 μg·ml^-1(r=0.999 8)范围内呈良好的线性关系,平均加样回收率分别为99.19%(RSD=0.9%)、98.44%(RSD=1.1%)、99.12%(RSD=1.0%)、99.18%(RSD=1.1%)(n=9)。结论:该方法简便、准确、重复性好,可用于黄连上清片的质量控制。     

HPLC波长切换法同时测定茵栀祛黄胶囊中7种成分的含量

摘 要 目的：建立HPLC波长切换法同时测定茵栀祛黄胶囊中栀子苷、甘草苷、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量。方法: 采用Waters Sunfire C18（250 mm×4.6 mm,5 μm）色谱柱;流动相：甲醇（A） 0.05%磷酸溶液（B）（梯度洗脱）,流速为1.0 ml·min^-1 ,柱温为25℃,检测波长(0~15 min：在238 nm波长下检测栀子苷和甘草苷;15~50 min：在254 nm波长下检测芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚),进样量为10 μl。结果: 栀子苷、甘草苷、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的线性范围分别为0.13～3.18 μg·ml^-1（r=0.999 8）、0.19～4.84 μg·ml^-1（r=0.999 7）、0.28～7.02 μg·ml^-1（r=0.999 9）、0.13～3.16 μg·ml^-1（r=0.999 9）、0.61～15.27 μg·ml^-1（r=0.999 9）、0.32～8.03 μg·ml^-1（r=0.999 9）、0.39～9.81 μg·ml^-1（r=0.999 9）;平均加样回收率分别为98.84%（RSD=0.74%）、99.34%（RSD=0.86%）、99.54%（RSD=0.30%）、99.56%（RSD=0.80%）、99.85%（RSD=0.41%）、99.57%（RSD=0.70%）、99.64%（RSD=0.30%）（n=9）。结论: 本文建立的HPLC含量测定方法,具有操作简便、专属性高、重复性良好、结果准确可靠的特点,可用于茵栀祛黄胶囊的质量控制。     

HPLC法同时测定大败毒胶囊中绿原酸、咖啡酸和阿魏酸的含量

摘 要 目的: 建立HPLC法同时检测大败毒胶囊中绿原酸、咖啡酸和阿魏酸的测定方法。方法: 采用Agilent C₁₈（250 mm×4.6 mm,5 μm）色谱柱;乙腈-0.4%磷酸溶液（15∶85）为流动相,流速：1.0 ml·min^-1;检测波长：324 nm。柱温:30℃,进样量：10 μl。结果:线性范围：绿原酸5.42～32.43 μg·ml^-1(r=0.999 8),咖啡酸2.63～26.32 μg·ml^-1(r=0.999 4),阿魏酸1.44～14.44 μg·ml^-1(r=0.999 9);平均回收率：绿原酸99.98%,RSD=0.2%(n=6),咖啡酸99.31%,RSD=0.4%(n=6),阿魏酸99.48%,RSD=0.8%(n=6)。结论:该方法操作简便、准确,重复性好,可用于测定大败毒胶囊中绿原酸、咖啡酸和阿魏酸的含量。     

HPLC-CAD法同时测定硫酸卡那霉素注射液中卡那霉素和卡那霉素B的含量

摘 要 目的：建立HPLC CAD法测定硫酸卡那霉素注射液中卡那霉素和卡那霉素B含量的方法。方法: 采用Boston Green ODS C18（250 mm×4.6 mm,5 μm）色谱柱,以0.2 mol·L-1三氟醋酸溶液 甲醇（95 ∶〖KG-*2〗5）作为流动相,流速:1.0 ml·min^-1,柱温:30℃,喷雾温度:55℃,喷雾压力:56.4 psi。结果:卡那霉素在0.385~38.500 μg·ml^-1之间呈现良好的线性关系（r=0.999 9）,检出限为0.075μg·ml^-1,定量限为0.154 μg·ml^-1,回收率为100.97%（n=9）。卡那霉素B在0.374~37.400 μg·ml^-1之间呈现良好的线性关系（r=1.000 0）,检出限为0.075 μg·ml^-1,定量限为0.150 μg·ml^-1,回收率为100.44%（n=9）。结论:建立的HPLC CAD测定卡那霉素和卡那霉素B含量的方法检出限低,操作简单准确,可以有效控制硫酸卡那霉素注射液的质量。     

HPLC法同时测定复方盐酸二甲双胍/沙格列汀渗透泵控释片的含量

摘 要 目的： 建立高效液相色谱法同时测定复方盐酸二甲双胍/沙格列汀渗透泵控释片的含量。方法: 采用UltimateXB-CN色谱柱（250 mm×4.6 mm,5 μm）,流动相为0.01 mol·L^-1磷酸二氢钾溶液（pH=4.7） 乙腈（15∶85）,检测波长为208 nm,流速为1.0 ml·min^-1,柱温为30℃,进样量20 μl。结果: 盐酸二甲双胍和沙格列汀分别在50.0～150.0 μg·ml^-1和0.5～1.5 μg·ml^-1浓度范围内与峰面积线性关系良好（r = 0.999 9和r=0.999 1）。平均回收率分别为99.5%和100.3%,RSD分别为0.56%和1.20%（n =9）。结论:该法专属性强,结果准确可靠,可用于复方盐酸二甲双胍/沙格列汀渗透控释片的质量控制。     

GC-MS法同时测定麝香保心丸中6种活性成分的含量

摘 要 目的：建立GC-MS法同时测定麝香保心丸中龙脑、异龙脑、肉桂醛、肉桂酸、麝香酮、苯甲酸苄酯6种活性成分的含量。方法: 采用气相色谱 质谱联用(GC MS)法,色谱柱为DB 5(30 m×0.25 mm, 0.1 μm)毛细管柱;程序升温：70℃恒温2 min,以5℃·min^-1)的速率升温至150℃,维持4 min,以20℃·min^-1)的速率升温至260℃,维持3 min;检测质荷比范围：10～425。结果: 龙脑、异龙脑、麝香酮、苯甲酸苄酯、肉桂醛、肉桂酸分别在0.022～22.000 μg·ml^-1(r=0.999 6),0.024～24.000 μg·ml^-1(r=0.999 6),0.028～28.000 μg·ml^-1 (r=0.999 8),0.034～34.000 μg·ml^-1 (r=0.999 6),0.040～40.000 μg·ml^-1 (r=0.999 7),0.050～50.000 μg·ml^-1 (r=0.999 9)范围内与峰面积呈良好的线性关系。龙脑、异龙脑、肉桂醛、肉桂酸、麝香酮、苯甲酸苄酯的平均加样回收率分别为97.20%,97.40%,97.53%,99.60%,98.78%和98.27%,RSD分别为0.89%,1.18%,1.52%,1.49%,0.79%和1.74%(n=6)。结论:该方法准确、有效、重复性好,可用于麝香保心丸多成分的质量控制研究。     

多波长HPLC法同时测定皮肤康洗液中5种有效成分的含量

摘 要 目的：建立多波长切换高效液相色谱法同时测定皮肤康洗液中芍药苷、甘草苷、甘草酸铵、大黄素和蛇床子素5种有效成分的含量。方法: 色谱柱为 Diamonsil C18柱(200 mm×4.6 mm,5 μm);流动相为乙腈 0.1%盐酸水溶液,梯度洗脱;流速为1.5 ml·min^-1;柱温为30℃;检测波长为232 nm(0～6 min,检测芍药苷)、277 nm(6～10 min,检测甘草苷)、254 nm(10 min以后,检测甘草酸铵、大黄素、蛇床子素）。结果: 芍药苷、甘草苷、甘草酸铵、大黄素和蛇床子素的线性范围分别为28.20～282.0 μg·ml^-1（r=0.999 7）、12.150～121.500 μg·ml^-1（r=0.998 8）、13.420～134.200 μg·ml^-1（r=0.999 5）、0.047～0.466 μg·ml^-1（r=0.999 9）、2.380～23.800 μg·ml^-1（r=0.999 9）,平均加样回收率分别为98.49%,99.00%,98.38%,97.36%,97.70%,RSD分别为0.71%,0.62%,0.85%,0.92%,0.78%（n=6）。结论:该方法简便、准确、灵敏度高、重复性好,可用于同时测定皮肤康洗液中上述5个有效成分的含量。     

HPLC法同时测定蒲药灌肠液中3个有效成分的含量

摘 要 目的： 建立蒲药灌肠液中香蒲新苷、异鼠李素-3-O-新橙皮苷和延胡索乙素的HPLC含量测定方法。方法: 采用ZORBAX SB-C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以乙腈-0.1%磷酸（三乙胺调节pH至6.0）为流动相,梯度洗脱程序,流速:1.0 ml·min^-1,检测波长为254 nm（0～14 min）和281 nm（14～25 min）,柱温:30 ℃。结果: 香蒲新苷、异鼠李素-3-O-新橙皮苷和延胡索乙素的线性范围分别为19.840～198.400 μg·ml^-1（r=0.999 6）、20.520～205.200 μg·ml^-1（r=0.999 8）和10.040～100.400 μg·ml^-1（r=0.999 7）,回收率分别为98.8%、98.6%和98.9%,RSD分别为1.4%、1.6%和1.3%（n=6）。结论: 该方法灵敏度高,专属性强,可用于蒲药灌肠液的质量控制。     

HPLC法测定枳实消痞丸中芸香柚皮苷、柠檬苦素、和厚朴酚及厚朴酚含量

摘 要 目的： 建立高效液相色谱法同时测定枳实消痞丸中芸香柚皮苷、柠檬苦素、和厚朴酚及厚朴酚含量的分析方法。方法: 色谱柱为岛津Shim-pack VP-ODS C18柱（250 mm×4.6 mm,5 μm）,流动相A为乙腈 甲醇(1∶2),流动相B为水,梯度洗脱,流速为1.0 ml·min^-1,柱温为30℃,进样量为20 μl;芸香柚皮苷检测波长为λ1=283 nm,柠檬苦素检测波长为λ2=210 nm,和厚朴酚、厚朴酚检测波长为λ3=294 nm。结果: 芸香柚皮苷、柠檬苦素、和厚朴酚、厚朴酚分别在5.26～105.20μg·ml^-1（r=0.999 8）、7.65～153.00 μg·ml^-1（r=0.999 4）、6.21～124.20 μg·ml^-1（r=0.999 3）、6.45～129.00 μg·ml^-1（r=0.999 6）范围内线性关系良好,平均加样回收率(n=6)分别为99.00％（RSD=0.77％）、98.17％（RSD=1.19％）、98.78％（RSD=0.86％）、97.90％（RSD=0.99%）。结论:该方法简便、准确、可靠,可用于枳实消痞丸的质量控制。     

化妆品中三种紫外吸收剂检测方法的建立

摘 要 目的：建立高效液相色谱法同时分析化妆品中亚苄基樟脑磺酸、樟脑苯扎铵甲基硫酸、4-甲基苄亚基樟脑这3种紫外吸收剂的方法。方法: 化妆品（水基、乳液类）经甲醇-乙腈-醋酸铵水溶液-四氢呋喃（30∶35∶30∶5,v/v）或者（膏霜、粉质类）经乙腈-甲醇-四氢呋喃（30∶20∶50, v/v）涡旋、超声提取后检测;采用Thermo scientific C18（250 mm×4.6 mm,5 μm）色谱柱,以甲醇、乙腈、0.02 mol·K^-1醋酸铵水溶液（冰醋酸调至pH 5.15）为流动相,梯度洗脱,柱温：35℃,流速：1.0 ml·min^-1 ,DAD 检测器,检测波长288 nm、300 nm。结果: 亚苄基樟脑磺酸、樟脑苯扎铵甲基硫酸、4 甲基苄亚基樟脑分别在12.26～98.06 μg·ml^-1（r=0.999 9）、9.31～74.48 μg·ml^-1（r=0.999 9）、6.86～54.88 μg·ml^-1（r=0.999 9）范围内呈良好的线性关系,检出限及定量限范围分别为4.6,6.4,1.6 ng和17.4,15.9,5.5 ng,平均回收率分别为99.2%（RSD=1.58%）、99.8%（RSD=2.38%）、99.2%（RSD=2.03%）（n=36）。结论:本方法简便快捷,重复性良好,结果准确可靠,适用于化妆品中紫外吸收剂的含量测定。     

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.