毛细管气相色谱法测定撒烈痛片含量

本文采用毛细管气相色谱法测定撒烈痛片的含量。色谱柱：交联ＳＥ－５４弹性石英毛细管柱（０．２５ｍｍｉｄ×２５ｍ），氢火焰离子化检测器（ＦＩＤ），进样量在０．３ｍｇ－１．３ｍｇ内４种成分与峰面积比呈直线相关（非那西丁：ｙ＝２．９５５４ｘ－０．１２８１，ｒ＝０．９９９５；咖啡因：ｙ＝１．５５８４ｘ－０．０２５７，ｒ＝０．９９９４；氨基比林：ｙ＝１．１６５３ｘ－０．０８９３，ｒ＝０．９９９２；苯巴比妥：ｙ＝２．５３５ｘ－０．１７５４，ｒ＝０．９９９８）。平均回收率±标准差分别为１００．２％±１．１７％、９９．８％±１．９４％、１００．５％±１．４６％、９８．４％±１．８２％。     

高效液相色谱法测定赖氨匹林颗粒剂含量及其降解产物水杨酸的控制

目的：采用高效液相色谱法测定赖氨匹林颗粒剂含量并对其降解产物水杨酸进行控制。方法：以Ａｌｌｔｉｍａ Ｃ１８柱为分析柱,甲醇－０．１％三乙胺溶液（１：１,冰醋酸调ｐＨ至３．５）为流动相,检测波长为２８０ｎｍ,以峰面积外标法计算。结果：赖氨匹林平均回收率为１００．０％,ＲＳＤ＝０．４７％（ｎ＝１１）;水杨酸平均回收率为１００．３％,ＲＳＤ＝１．１５％（ｎ＝６）。结论：本法简便、快速、结果准确、可靠。     

高效液相色谱法梯度法脱测定三七中三七皂苷R1含量

目的：以ＨＰＬＣ梯度法脱测定三七中三七皂苷Ｒ１含量。采用Ｓｐｈｅｒｉｃｏｒｂ ＮＨ２柱,流动相为ＣＨ３ＣＮ－ＣＨ３ＯＨ－Ｈ２Ｏ,梯度洗脱浓度５５：３０：１５→７０：２０：１０,波长２１０ｎｍ,外标一点法测定。结果：以峰面积计算,三七皂苷Ｒ１在５～４０μｇ．ｍｌ＾－１呈线性相关,γ＝０．９９４,最低检测限为０．６μｇ．ｍｌ＾－１（Ｓ／Ｎ）＝３。平均回收率１０２．６％,ＲＳＤ为１．４３％,日内误差ＲＳＤ＝１．７％（ｎ＝５）,日间误差ＲＳ＝３．０％（ｎ＝４）。结论：本法专属性强,结果准确,操作简便。     

反相HPLC法测定罂粟壳中吗啡,可待因的含量

采用Ｃ１８柱,以０．０５ｍｏｌ／Ｌ醋酸钠缓冲液（ｐＨ３．６）－乙腈－乙醇（２２：２：１）为流动相,检测波长为２５４ｎｍ。吗啡、可待因与各杂质成分分离度良好。含量测定的平均回收率分别为９４．７％（ＲＳＤ＝１．４３％,ｎ＝５）;９４．６％（ＲＳＤ＝１．７３％,ｎ＝５）。     

高效液相色谱法用于注射用穿琥宁及穿戛宁注射液含量测定的 …

目的：测定注射用穿琥宁及穿琥宁注射液含量。方法：采用高效液相色谱法。色谱柱为Ｓｈｉｍｐａｃｋ ＣＬＣ Ｃ１８柱,流动相为０．０２ｍｏｌ．Ｌ＾－１磷酸二氢钾（ｐＨ３．０）－乙腈－甲醇（４０：１０：５０）,流速１．２ｍＬ．ｍｉｎ＾－１,检测波长为２５１ｎｍ。应用二级管阵列检测器对色谱峰纯度进行检验,以排除有关物质的干扰。结果：平均回收率为９９．８８％,ＲＳＤ为０．１３％（ｎ＝３）。方法日内ＲＳＤ为０．     

反相高效液相色谱法同时测定苯巴比妥和卡马西平血药浓度

目的：建立同时测定微量血浆中苯巴比妥和卡马西平浓度的方法。方法：采用ＲＰ－ＨＰＬＣ法,以艾司唑仑为内标,同时测定微量血浆中苯芭巴比妥和卡马西平浓度。色谱柱ｓｈｉｍａｄｚｕ ｓｈｉｒｍｐａｃｋ ＣＬＣ－Ｃ１８不锈钢柱,流动相为醇－水（６０：４０）,流速０．８ｍｌ．ｍｉｎ＾－１,检测波长２５４ｎｍ。结果：苯巴比妥在４～６０μｇ．ｍｌ＾－１浓度范围内线性良好（ｒ＝０．９９９８）,卡马西平在２～１６μｇ．ｍｌ＾－１浓度范围内线性良好（ｒ＝０．９９９５）,最低检测限分别为１１．５７ｎｇ．ｍｌ＾－１和４．９２ｎｍ．ｍｌ＾－１,两者高、中、低３种浓度的平均回收率分别为９９．９２％,１０１．３０％,９７．９２％和９９．４１％,１０１．５２％,９８．２２％（ｎ＝９）,日内ＲＳＤ分别为３．１％,２．６％,３．８％和１．９％,１．６     

离子对色谱法测定颠茄及莨菪制剂中的3种有效成分

本文以安宫黄体酮为内标，采用离子对色谱法测定莨菪烷类的３种有效成分（东莨菪碱、山莨菪碱、阿托品）的含量。仪器：ＬＣ－４Ａ，层析柱：ＯＤＳ４．６ｍｍ×１５ｃｍ；柱温：３５℃；流动相：乙腈─甲醇─冰乙酸─二乙胺─水（水含０．００５ｍｏｌ／Ｌ十二烷基磺酸钠，５０：２５：０．０７５：０．１２５：２５）。在２０７ｎｍ波长处检测，样品回收率：东莨菪碱，１００．３％，ｎ＝５，ＲＳＤ＝１．３％；山莨菪碱，９８．８％，ｎ＝５，ＲＳＤ＝１．２％；阿托品，９９．１％，ｎ＝５，ＲＳＤ＝０．９３％。     

HPLC法测定复方福尔可定糖浆的含量

目的： 应用高效液相色谱法, 测定复方福尔可定糖浆的含量。方法： 采用ＯＤＳ 柱（２００ ｍ ｍ×４－６ ｍ ｍ） , 以０－０２ ｍｏｌ·Ｌ－ １ 庚烷磺酸钠甲醇溶液－ ０－０５ ｍｏｌ·Ｌ－ １ 磷酸二氢钾溶液－ 三乙胺（３０∶７０∶１ , 用磷酸调ｐＨ 为３－０） 为流动相, 检测波长为２１０ ｎｍ 。结果： 平均回收率（ ｎ ＝ ５） 福尔可定为９９－３ ％ , ＲＳＤ＝ ０－７ ％ ; 愈创木酚甘油醚为９９－８ ％ , ＲＳＤ＝ ０－５ ％ ; 盐酸麻黄碱为９９－５ ％ , ＲＳＤ＝ ０－４ ％ 。结论： 实验结果表明, 该方法简便, 准确, 灵敏度高, 重现性好。     

反相高效液相色谱法测定利凡诺的含量

报道了采用反相高效液相色谱法测定利凡诺的含量．色谱柱：Ｎｏｖａ－ＰａｈＣ１８柱；流动相：甲醇－乙腈－水（６０：３７：３），流动相中含有０．００５ｍｏｌ／Ｌ的ＰＩＣＢ－７（庚烷磺酸钠）试剂；检测波长：２７０ｎｍ。在０．３ｕｇ／ｍｌ～１．２５ｕｇ／ｍｌ范围内线性关系良好，０．５ｕｇ／ｍｌ和１ｕｇ／ｍｌ的利凡诺样品平均回收率分别为：１００．１３％（ＲＳＤ＝０．５３％）和９９．９９％（ＲＳＤ＝０．２９％）。本法最低检测限为１ｎｇ／ｍｌ，并且简便、快速、灵敏度高、专一性强，不受光解产物的影响。测定结果与中和法进行了比较。     

HPLC测定定晕宁颗粒中葛根素的含量

采用ＨＰＬＣ法,选用Ｓｙｍｍｅｔｒｙ－Ｃ１８柱和甲醇：水（２５：７５）,乙酸调ｐＨ４．２。测定定晕宁颗粒中葛根素含量,结果回归方程为Ｙ＝１．７７ｘ－０．２８１３,ｒ＝０．９９９（ｎ＝５）,线性范围为０．６１４￣６．１４μｇ,平均回收率为９９．０３％,ＲＳＤ为３．９８％。     

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.

---

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.