反相高效液相色谱法测定大青叶中腺苷的含量

目的建立大青叶中腺苷的含量测定方法。方法采用反相高效液相色谱法，固定相：Lichrosorb C18色谱柱(4.6 mm×150 mm，5 μm);流动相：甲醇 纯化水 冰醋酸(1∶96∶3);检测波长：257 nm;流速：0.8 mL·min ^-1;柱温：35 ℃。结果腺苷在1.52～48.64 μg·mL ^-1范围内线性关系良好(r＝0.999 2)，平均回收率分别为99.75%，RSD＝1.91%(n＝3);98.64%，RSD＝0.41%(n＝3);98.80%，RSD＝1.24%(n＝3)。结论该含量测定方法准确、快速、有效。     

甲硝唑凝胶的制备与质量标准研究

目的研究甲硝唑凝胶的制备与质量控制方法。方法用卡波姆等辅料配制甲硝唑凝胶。采用高效液相色谱法检查有关物质并测定甲硝唑的含量，色谱柱：Lichrosorb C18柱(4.6 mm×150.0 mm，5 μm)；流动相：甲醇 纯化水(15∶85)；流速：1 mL·min-1；检测波长：318 nm。 结果甲硝唑在18.6～148.8 μg·mL-1范围内线性关系良好，r＝0.999 95。甲硝唑平均回收率分别为99.7%，RSD＝1.38%(n＝3)；100.1%，RSD＝1.11%(n＝3)；98.8%，RSD＝0.20%(n＝3)。 结论用卡波姆等药用辅料可制备出理想的甲硝唑凝胶，制定的质量标准可达到质量控制的要求。     

复方双嘧达莫缓释片中阿司匹林和双嘧达莫的含量测定

目的建立同时测定复方双嘧达莫缓释片中阿司匹林和双嘧达莫含量的方法。方法采用反相高效液相色谱法，色谱柱：Alltech C18(4.6 mm×150 mm，5 μm)；流动相：甲醇-0.3%二乙胺水溶液-冰醋酸(45∶55∶4)；检测波长：235 nm；流速：1.2 mL·min^-1；柱温：30℃。 结果阿司匹林在635～101.60 μg·mL^-1范围内，峰面积与其浓度呈良好线性关系(r＝0.999 9，n＝6)，平均回收率为99.87%，RSD＝0.61%；双嘧达莫在18.7～299.2 μg·mL^-1范围内，峰面积与其浓度呈良好线性关系(r＝0.999 9， n＝6)，平均回收率为100.29%，RSD＝0.40%。3批自制复方双嘧达莫缓释片中阿司匹林和双嘧达莫相当于标示量的百分含量分别为：100.5%，100.4%，99.5%和100.9%，99.34%，100.3%。结论该法具有准确、简便、快速、灵敏且重现性好的特点，可用于复方双嘧达莫缓释片中阿司匹林和双嘧达莫含量的同时测定。     

布洛芬凝胶的制备与质量控制

目的制备布洛芬凝胶，并进行质量标准的研究。方法用卡波姆等辅料配制布洛芬凝胶，用高效液相色谱法测定布洛芬的含量并检查其有关物质；色谱柱：Lichrosorb C18柱(4.6 mm×150 mm，5 μm)；流动相：乙腈 水（58∶42）（用磷酸调节pH值至3.0），流速1 mL·min^-1，检测波长：264 nm。结果布洛芬在50.02～400.16 μg·mL^-1浓度范围内，线性关系良好(r＝0.999 9)；布洛芬平均回收率(n＝9)分别为99.0%(RSD＝0.44%)，100.5%(RSD＝0.56%)，99.2%(RSD＝0.35%)。结论用卡波姆等药用辅料可制备出理想的布洛芬凝胶，布洛芬凝胶的质量标准可靠。     

复方乳酸左氧氟沙星滴眼液的制备与含量测定

目的：研究复方乳酸左氧氟沙星滴眼液的制备及含量测定方法。方法：用紫外分光光度法和化学分析法对乳酸左氧氟沙星和地塞米松磷酸钠进行定性鉴别，用反相高效液相色谱法(RP HPLC)进行含量测定。以ODS C18分析柱(4.6 mm×250 mm，5 μm)为固定相，0.2%三乙胺水溶液(用磷酸调pH至2.7) 乙腈(68∶32)为流动相，检测波长240 nm，流速1.0 mL·min 1。结果：乳酸左氧氟沙星的线性范围12～60 μg·mL 1，r＝0.999 9，平均回收率99.66%，RSD＝1.9%(n＝5)。地塞米松磷酸钠的线性范围3～15 μg·mL 1，r＝0.999 1，平均回收率100.8%，RSD＝1.8%(n＝5)。结论：该制剂处方设计合理，制备方法可行，灵敏度高，测定结果准确，精密度良好。     

反相高效液相色谱法测定茵陈药材及其制剂中绿原酸含量

目的 建立测定茵陈药材及其制剂中绿原酸含量的高效液相色谱法。方法固定相：Kromasil C18 色谱柱(4.6 mm×250 mm,5 μm)；流动相：乙腈 0.1%磷酸（9：91）；检测波长：327 nm；流速：0.9 mL·min－1；柱温：40 ℃；进样量：10 μL。结果绿原酸在4.9～78.4 μg·mL－1浓度范围内线性关系良好（r＝0.999 7）；绿原酸平均回收率（n=3）分别为98.5%(RSD=1.32%)，99.0%(RSD=0.81%)，98.4%（RSD=0.52%）。结论 该方法灵敏快速、准确可靠，可作为茵陈药材及其制剂中绿原酸的质量控制方法。     

反相高效液相色谱法测定镇祛平口服液3种主要成分的含量

目的采用反相高效液相色谱法测定镇祛平口服液中盐酸曲普利定(C)、愈创甘油醚(G)和氢溴酸右美沙芬(D)3种主要成分的含量。方法色谱柱：YWG C18柱(150 mm×5 mm，10 μm)；流动相：770 mL甲醇 230 mL重蒸纯化水(含5 mmol·L 1庚烷磺酸钠，用磷酸调pH值为30)；在波长262 nm处进行检测。结果C在8594～77786 μg·mL 1，G在1888 ～1 6988 μg·mL 1，D在4108～36972 μg·mL 1浓度范围内线性关系良好。C的回收率＝ 999%，RSD＝080%；G的回收率＝1016%，RSD为069%；D的回收率＝1005%，RSD为068%。结论该法简便、快速、准确，可用于镇祛平口服液中3种主要成分的含量测定。     

阿莫西林钠含量测定方法的改进

目的：改进《中华人民共和国药典》中阿莫西林钠含量测定方法。方法：采用反相高效液相色谱法，色谱柱为Alltima C18柱(4.6 mm×150 mm，5 μm)，磷酸盐缓冲液(pH值5.0) 乙睛(96∶4)为流动相，检测波长254 nm，流速1.0 mL·min 1。结果：在0.026～0.520 mg·mL 1的浓度范围内线性关系良好，r＝0.999 8(n＝6)；平均回收率100.19%，RSD＝0.25%(n＝6)。结论：该法结果准确、可靠，重现性好。     

高效液相色谱法测定磷酸川芎嗪葡萄糖注射液中川芎嗪的含量

目的：探讨用高效液相色谱(HPLC)法测定磷酸川芎嗪葡萄糖注射液中川芎嗪的含量的方法。方法：采用Spherisorb C18色谱柱，以乙腈 0.02 mol·L 1磷酸二氢钾溶液(35∶65)为流动相；检测波长295 nm。结果：磷酸川芎嗪在12～28 μg·mL 1浓度范围内，浓度与峰面积呈良好的线性关系。平均回收率99.2%，RSD＝1.2%。结论：采用HPLC法测定磷酸川芎嗪含量灵敏性高，准确性和专属性好。     

联立方程组新解法测定银黄口服液的含量

目的：探讨不经分离直接测定银黄口服液中绿原酸及黄芩苷的含量的方法.方法：用联立方程组新解法,绿原酸在3～15 μg•mL 1浓度范围内线性关系良好,各自的平均吸收度(A)与浓度(C)的回归方程为：C＝ 18.197 0＋101.233 3A绿324(r＝0.999 9)；黄芩苷在6～30 μg•mL 1浓度范围内线性关系良好,回归方程为C＝ 28.074 3＋201.566 7A黄276(r＝0.999 9).结果：绿原酸平均回收率为100.22%,RSD为0.93%；黄芩苷平均回收率为100.17%,RSD为0.74%.结论：以联立方程组新解法测定银黄口服液中绿原酸与黄芩苷含量准确、快捷.     

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.