注射用甲磺酸培氟沙星近红外定量分析通用性模型的建立

摘 要 目的：利用近红外光谱法,建立注射用甲磺酸培氟沙星含量快速测定方法。方法: 采集注射用甲磺酸培氟沙星的近红外（NIR）光谱,以矢量归一化法对光谱进行预处理,选择谱段范围为9 176.2~8 169.5 cm^-1、6 051.9~5 716.3 cm^-1和4 509~3 999.9 cm^-1,回归方法为偏最小二乘法（PLS）,建立近红外定量模型。 结果: 经内部交叉验证建立预测模型,浓度范围为7.55%~77.69%,交叉验证均方根（RMSECV）为1.61%,相关系数为0.992 4。结论:建立的近红外定量分析模型可用于注射用甲磺酸培氟沙星快速定量分析。     

注射用磷霉素钠近红外定量分析通用性模型的建立

摘 要 目的： 利用近红外光谱法,建立注射用磷霉素钠含量快速检定方法。方法: 采集注射用磷霉素钠的近红外（NIR）光谱,建立近红外定量模型。结果: 以矢量归一化和多元散射校正法对光谱进行预处理、选择谱段范围为11 995.8～7 428.9及6 734.6～5 454 cm^-1,回归方法为偏最小二乘法。结论: 该近红外定量分析模型可用于注射用磷霉素钠快速定量分析。     

注射用阿莫西林钠/舒巴坦钠近红外快速定量分析模型的建立

摘 要 目的：利用近红外漫反射光谱（NIR）分析技术和化学计量学的方法,无损、快速的对注射用阿莫西林钠/舒巴坦钠进行定量分析。方法: 采集41批原始样品及20批破坏样品的近红外漫反射光谱,同时以法定方法分别测得阿莫西林、舒巴坦的含量,光谱预处理方法为一阶导数+矢量归一化,谱段范围为8 720 ～5 446 cm-1。结果: 以0.75 g规格的16批原始样品及15批破坏样品作为校正集经交叉验证建立定量模型,阿莫西林、舒巴坦的浓度范围分别为4.45%～61.82%、15.75%～30.25%,交叉验证均方根误差(RMSECV)分别为0.858、0.541,确定系数(R²) 分别为0.998 1、0.988 1;以0.75 g规格的5批原始样品及5批破坏样品作为验证集Ⅰ进行外部验证,预测均方根误差(RMSEP)为0.936、0.423;预测结果与法定方法参考结果对比,偏差均在1.5％之内;以1.5 g规格的10批原始样品及2批不同生产企业样品作为验证集Ⅱ,结果与法定结果一致,说明此模型通用于两种规格、适用性强。结论: 此方法快速、可靠,可在安瓿瓶外无损采集光谱,可用于药品的快速定量分析。     

拉曼光谱法快速测定注射用更昔洛韦的含量

摘 要 目的：建立一种利用拉曼技术快速测定注射用更昔洛韦的方法。方法: 运用拉曼光谱技术对注射用更昔洛韦进行含量测定,并与HPLC法进行比较。拉曼光谱条件：采用光纤自动测量模式,探头焦距为5 mm,激发光源为785 nm,分辨率为4 cm^-1,测试时间为100 s,激光输出功率为400 mW,扫描范围为3 000～200 cm^-1,检测器工作温度为-50℃。结果: 更昔洛韦在2.5～50.0 mg·mL^-1浓度范围内与1 475 cm^-1峰位的峰面积呈良好的线性关系（r=0.998 0）,平均回收率为99.47%（RSD=1.02%,n=9）。结论:拉曼光谱法快捷、简便,可用于注射用更昔洛韦含量的快速测定。     

片姜黄中挥发油含量近红外定量检测模型的建立

摘 要 目的：建立片姜黄近红外定量检测模型,快速测定片姜黄中挥发油的含量。方法: 以中国药典中蒸馏法测定片姜黄中挥发油的含量,然后采用傅立叶变换近红外光谱技术并结合偏最小二乘法（PLS）建立、优化模型,采用校正模型的相关系数（r）、校正均方根误差（RMSEC）、内部交叉验证均方根误差（RMCECV）和预测模型相关系数（r）、预测均方根误差（RMSEP）对校正模型进行评价。结果: 选择谱段为7 189～4 227 cm-1、8 813～7 478 cm-1,以二阶导数＋MSC对原始光谱进行预处理建立定量分析模型;所建立的片姜黄挥发油定量校正模型中的r为0.976 9;RMSEC为0.090 7;RMCECV为0.377 3;片姜黄挥发油预测模型的r值为0.905 3;RMSEP为0.196 0。结论: 建立的近红外定量模型预测精度较高,可用于片姜黄挥发油含量的快速测定。     

近红外光谱法快速测定注射用乙酰谷酰胺水分

摘 要 目的：利用近红外光谱(NIR)技术结合化学计量学方法对注射用乙酰谷酰胺的水分进行快速定量分析。方法: 以51批注射用乙酰谷酰胺及7批加速引湿样本为分析对象,采用卡尔费休法测定样品水分;采集样品近红外光谱,选择建模谱段为5 419.1～4 993.1 cm-1,光谱预处理方法为一阶导数+多元散射校正,利用偏最小二乘法建立定量模型。结果: 建模样本水分值范围为0.8%～5.9%,交叉验证均方根误差为0.144,相关系数为0.982 4;外部验证均方根误差为0.155,相关系数为0.983 7。结论: 建立的模型能对注射用乙酰谷酰胺的水分进行快速定量分析,方法简单可靠,可用于药品的现场快速分析。     

表面增强拉曼光谱法检测保健品中添加的微量西布曲明

摘 要 目的： 对保健品中添加的西布曲明进行快速检测。方法: 用便携式拉曼光谱仪对市场上几种添加了微量西布曲明的保健品进行快速检测,实验条件：激发波长: 785 nm±0.5 nm,光谱覆盖范围: 175～3 100 cm^-1,信号采集时间20 s,光谱分辨率: 8 cm^-1。结果: 研究表明, 表面增强拉曼光谱法可快速检测出添加于保健品中的微量西布曲明,检测结果与传统方法检测的结果相吻合。结论:该方法快速、简便、无损,可作为检测保健品中非法添加的微量西布曲明的快检方法。     

硝苯地平缓释片（II）近红外快速检验模型的建立与验证

目的 建立硝苯地平缓释片（II）近红外一致性检验模型和快速定量模型。方法 使用近红外漫反射光谱（NIR）技术并采用化学计量学方法,选择9 000～7 500 cm^-1、6 900～5 600 cm^-1和5 000～4 250 cm^-1的谱段和二阶导数+矢量归一化的预处理方法建立一致性检验模型;选择7500～9750 cm^-1的谱段和直线差减法建立一致性检验模型。结果 对收集的6批样品建立一致性检验模型并通过了模型验证;以3批原始样品及6批模拟样品作为校正集建立定量模型经交叉验证,硝苯地平的浓度范围为0.018 60～0.091 09 mg·mg^-1,均方根误差(RMSECV)为0.001 95,确定系数(R²)为0.992 9;再以3批原始样品作为验证集进行外部验证,预测均方根误差(RMSEP)为0.000 531;预测结果与法定方法测得含量结果对比,偏差在1.5％之内。结论 所建模型准确、高效,厂家可用于在线质量监控、快速定量分析,监管部门可用于筛查、打击假劣药品。     

HPLC-ELSD法测定复方金刚烷胺氨基比林片中氨基比林和盐酸金刚烷胺的含量

摘 要 目的：建立一种测定复方金刚烷胺氨基比林片中氨基比林和盐酸金刚烷胺含量的HPLC ELSD法。方法: 色谱柱：Aglient Eclipse Plus C18 柱（250 mm×4.6 mm,5 μm）;流动相：0.1%的三氟醋酸溶液 乙腈(85∶15);流速：0.7 ml·min^-1;柱温：室温;蒸发温度：40℃;雾化温度：40℃;载气（氮气）流速：1.8 L·min^-1,进样量：10 μl。结果: 氨基比林和盐酸金刚烷胺分别在606.72～3 033.60 μg·ml^-1、400.96～2 004.80 μg·ml^-1范围内峰面积与进样量的对数呈现良好的线性关系（r分别为0.999 7、0.999 4）;平均回收率分别为99.5%、99.3%,RSD分别为0.35%、0.40%（n=9）。结论:该方法简便、快速、准确、重复性好,适用于复方金刚烷胺氨基比林片中氨基比林和盐酸金刚烷胺的含量测定。     

近红外光谱法对非洛地平缓释片一致性检验研究

摘 要 目的： 建立3个厂家的非洛地平缓释片近红外光谱法一致性检验模型,考察制剂工艺的差别,通过稳健、准确、代表性强的近红外一致性模型实现非洛地平缓释片的快速检验和筛查。 方法: 对评价性抽验抽取的6个厂家中的3个建立非洛地平缓释片近红外一致性检验模型,选取4 000～9 000 cm^-1区段为建模区段、一阶导数+矢量归一化法作为预处理方法。结果:建立了3个厂家非洛地平缓释片的近红外一致性模型,对抽样的6个企业样品进行了预测,对本厂产品和其他厂家产品的预测成功率均为100%。结论: 近红外光谱法能够用于快速鉴别不同厂家的非洛地平缓释片,对制剂工艺进行考察。     

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.

     

In vitro studies on sterically stabilized liposomes (SL) as enzyme carriers in organophosphorus (OP) antagonism

This study describes a new approach for organophosphorous (OP) antidotal treatment by encapsulating an OP hydrolyzing enzyme, OPA anhydrolase (OPAA), within sterically stabilized liposomes. The recombinant OPAA enzyme was derived from Alteromonas strain JD6. It has broad substrate specificity to a wide range of OP compounds: DFP and the nerve agents, soman and sarin. Liposomes encapsulating OPAA (SL)* were made by mechanical dispersion method. Hydrolysis of DFP by (SL)* was measured by following an increase of fluoride ion concentration using a fluoride ion selective electrode. OPAA entrapped in the carrier liposomes rapidly hydrolyze DFP, with the rate of DFP hydrolysis directly proportional to the amount of (SL)* added to the solution. Liposomal carriers containing no enzyme did not hydrolyze DFP. The reaction was linear and the rate of hydrolysis was first order in the substrate. This enzyme carrier system serves as a biodegradable protective environment for the recombinant OP-metabolizing enzyme, OPAA, resulting in prolongation of enzymatic concentration in the body. These studies suggest that the protection of OP intoxication can be strikingly enhanced by adding OPAA encapsulated within (SL)* to pralidoxime and atropine.     

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.     

Steroidal sapogenin contents in some domestic plants

In order to find out the values of the steroid resources for the future use. the compositions and contents of steroidal sapogenins from 13 domestic plants have been investigated. As a result,Dioscorea nipponica, D. quinqueloba andSmilax china were found to have large amount of diosgenin. And pennogenin inTrillium kamtschaticum andParis verticillata, yuccagenin inAllium fistulosum, hecogenin inAgave americana and neochlorogenin inSolanum nigum were appeared to be major steroidal sapogenins.