HPLC测定盐酸贝那普利片的含量

目的　测定盐酸贝那普利片中贝那普利的含量。方法　采用HPLC ,ZorbaxXDB -C18色谱柱 (5 μm ,4 .6mm× 15 0mm) ,柱温 2 5℃ ,流动相为 0 .0 75 %HAc -甲醇 (35∶6 5 ) ,流速 1.0ml·min-1;DAD检测波长 2 39nm。结果　贝那普利浓度在 0 .8～ 4 8g·ml-1范围内线性关系良好 ,最低检测浓度为 0 .4 μg·ml-1,日内RSD≤ 1.5 1% ,日间RSD≤ 1.6 9% (n =5 ) ,回收率 98.9%～99 .9% (n =5 )。结论　所用方法简便快速 ,准确可靠 ,可用于盐酸贝那普利片的含量测定。     

国产盐酸贝那普利片质量评价

目的：评价国产盐酸贝那普利片的质量现状。方法：采用法定标准方法和探索性研究对盐酸贝那普利片进行相关测定。结果：93批样品依据法定标准检验合格率为100%。不同生产企业产品之间有关物质和溶出度存在差异。结论：目前国内生产的盐酸贝那普利片产品质量符合法定标准,但探索性研究提示部分生产企业的生产工艺值得改进,改善制剂的溶出行为,减少有关物质的总杂质量。     

高效液相色谱法测定普利沙星片含量及有关物质

目的采用高效液相色谱法建立普利沙星片含量及有关物质的测定方法。方法色谱柱：Hypersil C18 (5 μm，4.6 mm×250 mm)，流动相：乙腈 0.1%磷酸-1 mol·L-1戊烷磺酸钠溶液（31∶69∶0.2），流速：0.8 mL·min-1，检测波长：276 nm，柱温：（35.0±0.1）℃。结果制剂中辅料对普利沙星测定无干扰，普利沙星与有关物质完全分离，酸、碱及氧破坏均有降解产物生成，降解产物能够与普利沙星分离，不干扰测定。在5～500 μg·mL-1浓度范围内，峰面积（A）与浓度（C）线性关系良好，r＝0.999 9；平均回收率99.40%（n＝9）；日内，日间精密度RSD＜0.5%；溶液室温放置24 h稳定（RSD＜0.5%）。结论该方法简便，准确，重现性好，专属性强，可用于普利沙星片的含量及有关物质测定。     

HPLC法测定复方贝母片中盐酸麻黄碱和盐酸伪麻黄碱的含量

目的：建立复方贝母片中盐酸麻黄碱和盐酸伪麻黄碱的含量测定方法。方法：采用Agilent TC C18（4.6×250mm,5μm）色谱柱,以乙腈-0.1%磷酸溶液（3：97）为流动相;流速1.0ml·min-1,柱温30℃,检测波长为207 nm。结果：盐酸麻黄碱在0.041 5～1.245 6 μg范围内线性关系良好（r=0.999 9）,盐酸伪麻黄碱在0.020 6～0.618 6 μg范围内线性关系良好（r=0.999 9）,平均回收率分别为96.7%、95.3%,RSD分别为1.3% 、1.6%（n=6）。3批样品的含量测定结果分别为：盐酸麻黄碱0.121～0.129mg·片-1,盐酸伪麻黄碱0.104～0.109mg·片-1。结论：本方法简便、准确,重现性好,可以用于复方贝母片的质量控制。     

HPLC梯度洗脱法同时测定复方盐酸喹那普利／氢氯噻嗪片剂含量及有关物质

目的：建立HPLC法,同时测定复方盐酸喹那普利／氢氯噻嗪片剂中的主成分及其有关物质。方法：色谱柱为LichrospherC,8柱（250mm×4．6mm,5μm）;流动相为乙腈-0．05％三乙胺水溶液（用磷酸调pH至3．50）,梯度洗脱;柱温为40℃;检测波长为215nm。主成分测定采用外标法,有关物质检查采用主成分1％自身对照法。结果：两主成分与其有关物质等5种化合物均能较好分离,相邻各峰间分离度均大于1．5;盐酸喹那普利和氢氯噻嗪的线性范围分别为0．708—63．72mg·L-1（r=0．9998）和0．758～68．22mg·L-1（r=0．9999）;复方片剂中盐酸喹那普利与氢氯噻嗪的含量均为标示量的95％～105％,有关物质含量均小于或等于0．8％。结论：本法简便快速、专属性强、灵敏度高、重复性好,可用于该复方片剂的含量测定和杂质检查。     

HPLC法测定复方盐酸贝那普利片中盐酸贝那普利和苯磺酸氨氯地平的含量

目的建立复方盐酸贝那普利片中盐酸贝那普利和苯磺酸氨氯地平含量测定的HPLC法。方法采用Diamonsil C18柱(200 mm×4.6 mm,5μm);流动相为氯化钾溶液(1 000 mL中含90 mmoL氯化钾和10 mmoL盐酸,pH值2.06)-水-甲醇(体积比为17∶25∶58),每1 000 mL流动相中加入612 mg高氯酸钠;流速为1 mL.min-1;检测波长为240 nm;柱温为35℃;进样量为20μL。结果盐酸贝那普利与苯磺酸氨氯地平可达到较好分离,盐酸贝那普利的质量浓度在10.0～200.0mg.L-1内与峰面积呈良好的线性关系(r=0.999 8);苯磺酸氨氯地平(按氨氯地平计)质量浓度在5～100 mg.L-1内与峰面积呈良好的线性关系(r=0.999 8)。盐酸贝那普利与苯磺酸氨氯地平的平均回收率分别为99.9%(n=9)和100.4%(n=9)。结论 HPLC法适用于复方盐酸贝那普利片中盐酸贝那普利和苯磺酸氨氯地平的含量测定。     

补阳还五汤联合盐酸贝那普利治疗早期糖尿病肾病

目的：观察补阳还五汤联合盐酸贝那普利治疗早期糖尿病肾病的临床疗效。方法：将60例确诊为早期糖尿病肾病的患者随机分为两组。治疗组给予中药补阳还五汤原方合盐酸贝那普利片治疗,对照组给予盐酸贝那普利片治疗,疗程均为8周。结果：①两组治疗后,中医症状疗效比较,治疗组30例,有效率93.33%;对照组30例,有效率70.00%;②两组治疗后西医疗效（实验室检查）比较,治疗组有效率90.00%,对照组有效率63.33%。结论：补阳还五汤联合盐酸贝那普利治疗早期糖尿病肾病值得临床推广。     

反相高效液相色谱法测定盐酸氨溴索注射剂的含量

目的应用反相高效液相色谱法测定盐酸氨溴索注射液中主成分及有关物质的含量。方法 Hypersil C18色谱柱（4.6 mm×150 mm，5 μm），流动相为0.175%磷酸氢二铵水溶液(pH值7.3)-乙腈（52∶48），流速：1.0 mL·min^-1，柱温：40℃，检测波长：248 nm。结果线性范围为20.176～100.880 μg·mL^-1，r＝0.999 9。结论该测定方法简便、准确，可用于盐酸氨溴索注射液的有关物质检查及含量测定。     

近红外光谱法快速测定盐酸贝那普利片的含量

目的利用近红外漫反射光谱技术快速测定盐酸贝那普利片的含量。方法采集盐酸贝那普利片NIR光谱,采用偏最小二乘法（PLS）进行回归,通过建立NIR光谱与理论测定值之间的多元校正模型,测定盐酸贝那普利片的含量。结果定量分析模型浓度范围为2.53%~6.55%（mg/mg）;内部交叉验证均方差（RMSECV）为0.138,决定系数（R2）为98.47%;外部验证均方差（RMSEP）为0.137,决定系数（R2）为98.76%,平均绝对偏差为0.11%（mg/mg）,平均相对偏差为2.49%。结论该方法准确可靠、快速简便,可以满足药品现场快速检测的需要。     

盐酸氨溴索注射液降解杂质结构与降解途径分析

目的：对盐酸氨溴索注射液在氧化和光照条件下强制破坏产生降解杂质的结构和来源进行研究。方法：通过对盐酸氨溴索注射液在各条件下进行强制破坏,产生降解杂质,采用VisionHT C18色谱柱（250 mm × 4.6 mm,5 μm）。以0.01 mol·L-1磷酸氢二铵溶液（用磷酸调节pH至7.0）-乙腈（50∶50）洗脱,分离制备有关物质,采用质谱法,对主要降解产物的结构进行研究。归属杂质来源,推测形成路径。结果：确定了盐酸氨溴索注射液中8个降解杂质的分子结构,并明确了其质谱裂解反应机理。结论：成功推测了盐酸氨溴索注射液强制氧化和光降解产物的结构,并阐明其产生的路径。     

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.