HPLC法测定不同产地垂盆草药材中木犀草苷的含量

摘 要 目的： 建立反相高效液相色谱法测定垂盆草药材中木犀草苷的含量。方法: 采用Waters SymmetryShield C₁₈ (250 mm×4.6 mm,5 μm) 色谱柱;以四氢呋喃 甲醇 水 磷酸（9〖KG*9〗∶〖KG-*2〗17〖KG*9〗∶〖KG-*2〗74〖KG*9〗∶〖KG-*2〗0.25）为流动相,流速为1.0 ml·min^-1,检测波长为350 nm,柱温为35℃,进样量为10 μl。结果: 木犀草苷在5.2～208.0μg·mL^-1（r=0.999 9）范围内呈现良好的线性关系;平均回收率为99.12％,RSD=0.94%（n=6）。结论:该方法简便、灵敏、准确、专属性强,重复性好,可作为垂盆草药材中木犀草苷含量测定的方法。     

顶空气相色谱法测定盐酸厄洛替尼中有机溶剂残留量

摘 要 目的：建立顶空毛细管气相色谱法测定盐酸厄洛替尼中有机溶剂残留量的方法。方法: 采用顶空毛细管气相色谱法,色谱柱为DB 624毛细管柱（30 m×0.53 mm,3.0 μm）,载气为氮气,流速为2.0 ml·min^-1,进样口温度为190 ℃,FID检测器温度为230 ℃,采用程序升温：初始温度为35 ℃,保持8 min,以28 ℃·min^-1升温至170 ℃,保持8 min,再以32 ℃·min^-1升温至200 ℃,保持7 min。顶空瓶平衡温度为100 ℃,时间30 min。结果: 乙醇、异丙醇、二氯甲烷、正丁醇分别在0.68~409.14 μg·mL^-1（r=0.999 8）、0.67~404.88 μg·mL^-1（r=0.999 8）、1.71~51.31 μg·mL^-1（r=0.999 7）、0.72~431.12 μg·mL^-1（r=0.999 8）浓度范围内线性关系良好,平均回收率分别为99.0%（RSD=0.41%,n=9）、100.2%（RSD=0.52%,n=9）、97.1%（RSD=1.75%,n=9）、102.5%（RSD=1.08%,n=9）。结论:该方法简便、准确性好,适用于盐酸厄洛替尼中4种有机溶剂残留量的测定。     

离子色谱法测定羟苯乙酯中氯离子和硫酸根离子及不同级别产品质量状况的评价

摘 要 目的：建立离子色谱法同时测定羟苯乙酯中氯离子和硫酸根离子的含量,评价不同级别羟苯乙酯中氯离子和硫酸根离子含量的质量状况。方法: 采用色谱柱为Dionex IonPac AS18 (250 mm×4 mm,5 μm),流动相为氢氧化钾淋洗液（梯度洗脱）,流速为1.0 ml·min-1,进样量为25 μl。结果: 氯离子和硫酸根离子分别在0.02～4.00 μg·ml-1、0.10～10.00 μg·ml-1范围内线性关系良好（r分别为0.999 9和0.999 5）,氯离子和硫酸根离子回收率分别为90.12%、85.54%,RSD分别为6.2%、3.4%（n=9）。63批样品中,氯离子和硫酸根离子含量分别为0.000 3%～0.015 7%、0.000 9%～0.024 4%。结论: 该方法操作简便、快速,结果准确,可用于同时测定羟苯乙酯中氯离子和硫酸根离子的含量,为其质量控制提供保证。     

HPLC法测定柏石水调散中盐酸巴马汀和盐酸小檗碱的含量

摘 要 目的：建立HPLC方法同时测定柏石水调散中盐酸巴马汀和盐酸小檗碱含量。方法: 采用反相离子对高效液相色谱法,色谱柱为Agilent Zorbax SB C18（150 mm×4.6 mm,5 μm）;流动相为乙腈 0.1%磷酸溶液（50〖KG*9〗∶〖KG-*2〗50）（每100 ml加十二烷基硫酸钠0.2 g）;流速为1.0 ml·min-1;检测波长为345 nm;进样量为10 μl;柱温为室温。结果: 盐酸巴马汀和盐酸小檗碱进样量分别在1.11~22.16 μg·mL^-1（r=0.999 6）和2.11~42.24 μg·mL^-1（r=0.999 8）范围内与峰面积线性关系良好,平均回收率分别为98.94%和101.3%,RSD分别为2.43%和2.05%（n = 6）。结论: 本方法快速、简便、准确,可用于柏石水调散中盐酸巴马汀和盐酸小檗碱的含量测定。     

HPLC法同时测定泻肝安神丸中龙胆苦苷、栀子苷、黄芩苷的含量

摘 要 目的：建立HPLC法同时测定泻肝安神丸中龙胆苦苷、栀子苷、黄芩苷的含量。方法: 采用Phenomenex Luna C18(2)柱（250 mm×4.60 mm,5 μm）,以甲醇－0.2%磷酸溶液为流动相,梯度洗脱,流速为1.0 ml·min^-1,柱温为30℃,检测波长为254 nm,进样量为10 μl。结果: 龙胆苦苷在10.55~168.80 μg·mL^-1范围内线性关系良好（r=0.999 9）,平均回收率为98.68％,RSD为1.2％（n=6）;栀子苷在29.85~477.60 μg·mL^-1范围内线性关系良好（r=0.999 8）,平均回收率为98.76％,RSD为1.1％（n=6）;黄芩苷在43.05~688.80 μg·mL^-1范围内线性关系良好（r=0.999 7）,平均回收率为98.36％,RSD为1.4％（n=6）。结论:该方法简单、准确,可同时测定3种成分的含量,可用于泻肝安神丸的质量控制。     

HPLC法同时测定复合维生素B片中5种维生素的含量

摘 要 目的：应用HPLC技术,建立同时测定复合维生素B片中维生素B1（硫胺素）、维生素B2（核黄素）、维生素B3（烟酰胺）、维生素B5（泛酸）和维生素B6（吡多辛）含量的方法。方法: 采用Alltima C18色谱柱（250 mm×4.6 mm, 5 μm）,以50 mmol·L^-1磷酸二氢铵溶液（磷酸调至pH 3.0） 乙腈为流动相,梯度洗脱,流速为0.5 ml·min^-1,维生素B1、维生素B2、维生素B3、维生素B6的检测波长为275 nm,维生素B5的检测波长为210 nm,柱温30℃,进样量为5 μl。结果:维生素B1、维生素B2、维生素B3、维生素B5和维生素B6的线性范围分别为39.48～197.40μg·mL^-1、40.16～200.80 μg·mL^-1、39.36～196.80 μg·mL^-1、38.80～194.00 μg·mL^-1、41.76～208.80 μg·mL^-1,r均≥0.999 9。其平均回收率分别为98.70%,99.91%,99.04%,99.63%,98.75%,RSD分别为0.40%,0.27%,0.40%,0.92%,0.39%（n=9）。结论:该方法准确、简便、快速,可作为复合维生素B片中维生素B1、维生素B2、维生素B3、维生素B5和维生素B6同时测定的方法。     

HPLC法测定吲哚美辛呋喃唑酮栓中两组分的含量

摘 要 目的：建立同时测定吲哚美辛呋喃唑酮栓中两组分含量的HPLC法。方法: 采用XTerra RP18色谱柱(250 mm×4.6 mm,5 μm),以甲醇为流动相A,0.01 mol·K^-1磷酸二氢钾溶液 三乙胺(100〖KG*9〗∶〖KG-*2〗0.02)为流动相B,梯度洗脱,流速1.0 ml·min^-1,柱温30 ℃,检测波长263 nm,进样量10 μl。结果: 吲哚美辛呋喃唑酮栓中呋喃唑酮和吲哚美辛的分离度符合要求;线性范围分别为5.12~81.87 μg·ml^-1 (r=1.000 0)和3.78~60.45 μg·ml^-1 (r=1.000 0);平均回收率分别为99.6% (RSD=1.5%,n=6)和100.3% (RSD=1.6%,n=6);定量限分别为0.02 μg·ml^-1和0.05 μg·ml^-1。结论:该法经方法学验证,适用于吲哚美辛呋喃唑酮栓的质量评价。     

小儿至宝丸中朱砂和雄黄的含量测定

摘 要 目的： 建立小儿至宝丸中朱砂和雄黄的含量测定方法。方法: 分别采用原子吸收分光光度法（AAS）和电感耦合等离子体发射光谱法（ICP-AES）测定小儿至宝丸朱砂中的汞和雄黄中的砷含量。结果: AAS法测定的汞的线性范围为5～100 μg·mL^-1（r=0.999 9）,砷的线性范围为2～50 μg·mL^-1（r=0.999 2）,汞的平均回收率为99.3%,RSD为3.0%（n=6）,砷的平均回收率为104.5%,RSD为2.1%（n=6）;ICP AES法测定的汞的线性范围为0.1～20.0 μg·mL^-1（r=0.999 97）,砷的线性范围为0.1～20.0 μg·mL^-1（r=0.999 99）,汞的平均回收率为96.6%,RSD为1.4%（n=6）,砷的平均回收率为104.1%,RSD为1.1%（n=6）。结论:本文建立的方法准确、专属性强,可用于控制小儿至宝丸中毒性成分的含量。     

HPLC法测定姜黄素-槲皮素复方自微乳的载药量和包封率

摘 要 目的：建立HPLC法测定姜黄素 槲皮素复方自微乳（CUR-QUE-SMEDDS）的载药量和包封率。方法: 采用离心法分离游离药物,HPLC法测定药物含量。色谱柱：Purospher STAR LP C18 柱（250 mm×4.6 mm,5 μm）,流动相：乙腈 4%冰醋酸（50∶50）,流速：1.0 ml·min^-1,检测波长：370 nm,柱温：30℃,进样量：10 μl。结果: 姜黄素和槲皮素的线性范围分别为10.728~96.552 μg·mL^-1（r=0.999 8）和1.08~9.72 μg·mL^-1（r=0.999 9）,平均回收率分别为99.98%（RSD=1.46%,n=9）和100.34%（RSD=1.06%,n=9）。CUR QUE SMEDDS中姜黄素和槲皮素的包封率分别为（95.97±0.50）% 和（95.91±2.52）%,载药量分别为（25.82±0.15）mg·g^-1和（1.80±0.05）mg·g^-1。结论:该法准确可靠,快速简便,适用于测定CUR-QUE-SMEDDS的载药量和包封率。     

气相色谱法测定牛黄清心丸（局方）中龙脑和异龙脑含量

摘 要 目的：建立气相色谱法测定牛黄清心丸（局方）中龙脑和异龙脑含量的方法。方法: 采用HP INNOWAX毛细管柱（30 m×0.25 mm,0.25 μm）,柱温110 ℃,进样口温度200 ℃;FID检测器温度230 ℃;载气为氮气;载气流速1.8 ml·min^-1,分流比10∶1;进样量：1 μl。结果:龙脑和异龙脑分别在0.01～5.09 μg·ml^-1（r=0.999 5）和0.01～5.03 μg·ml^-1（r=0.999 1）范围内线性关系良好,平均回收率分别为99.34%和99.24%,RSD分别为0.59%和0.62% （n=6）。结论:所建方法准确、灵敏、简便,可用于牛黄清心丸（局方）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.

     

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.