反相高效液相色谱法同时测定补阳还五汤中芍药苷和阿魏酸的含量

目的采用反相高效液相色谱法测定补阳还五汤中的芍药苷和阿魏酸的含量。方法固定相选用Symmetry C18柱（4.6 mm×150 mm，5 μm）；流动相为1%醋酸 甲醇（70∶30）(pH值为3.15)；流速：1.0 mL·min^-1；柱温：30 ℃；检测波长：芍药苷230 nm，阿魏酸320 nm。结果芍药苷和阿魏酸含量测定线性范围分别是4～24 μg·mL^-1，0.4～2.0 μg·mL^-1，r分别是0.999 9，0.999 8，平均加样回收率分别是101.72%（RSD＝0.27%，n＝3），104.72%（RSD＝0.46%，n＝3）。结论该检测方法简便，结果准确，可用于该方剂的质量控制。     

高效液相色谱法测定十滴水中大黄素和大黄酚的含量

目的建立高效液相色谱（HPLC）法测定十滴水中大黄素和大黄酚含量的方法。方法Diamonsil C18柱(4.6 mm ×250 mm，5 μm)，甲醇-0.3%磷酸溶液（85∶15）为流动相，检测波长254 nm，柱温室温，进样量，10 μL。结果大黄素和大黄酚浓度分别在2.20～35.20 μg·mL^-1（r＝0.999 9）和2.11～67.58 μg·mL^-1（r＝0.999 9）与峰面积线性关系良好，平均回收率分别为97.47%（RSD＝1.74%，n＝5）和97.77%（RSD＝1.57%，n＝5）。结论该法操作简便，结果准确，可用于十滴水的质量控制。     

高效液相色谱法测定菝葜醋酸乙酯提取物中白藜芦醇的含量

目的建立高效液相色谱法测定菝葜醋酸乙酯提取物中白藜芦醇含量的方法。方法Zirchrom Kromasil C18 色谱柱(4.6 mm×250 mm，5 μm)；流动相：乙腈-水(30∶70)；流速：1.0 mL·min^-1；柱温：室温；检测波长303 nm。结果白藜芦醇对照品线性范围18.8～94.0 μg·mL^-1，r＝0.999 6(n＝5)，样品平均回收率为101.10 %，RSD＝0.64 %(n＝5)，菝葜醋酸乙酯提取物中白藜芦醇的平均含量为29.59 μg·mg^-1。结论该方法简便、快捷、重现性好，为菝葜醋酸乙酯提取物的质量控制提供依据。     

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。     

高效液相色谱法测定复方丹参片中丹酚酸B和丹参酮ⅡA的含量

［摘要］目的 建立高效液相色谱（HPLC）法同时测定复方丹参片中丹酚酸B和丹参酮ⅡA的含量. 方法 色谱柱：Hypersil ODS（4.6 mm×250 mm,5 μm）;用甲醇-乙腈-0.1%磷酸梯度洗脱作为流动相;流速：0.9 mL·min^-1;检测波长：270 nm;柱温：40 ℃;进样量：10 μL. 结果 丹酚酸B在24.2～242.0 μg·mL^-1,丹参酮ⅡA在5.25～52.50 μg·mL^-1的浓度范围内线性关系良好,丹酚酸B的平均回收率为98.2%（RSD=0.92%,n＝3）,丹参酮ⅡA的平均回收率为98.4%（RSD=0.97%,n＝3）.结论 该方法灵敏快速、准确可靠,可作为复方丹参片的质量控制方法.     

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。     

HPLC同时测定疗筋涂膜剂中5种大黄成分的含量

目的 建立高效液相色谱法同时测定疗筋涂膜剂中5种成分的含量。方法 采用Hypersil ODS-C₁₈柱(250 mm × 4.6 mm,5 μm) , 甲醇-0.05％磷酸(85∶15)为流动相,流速：0.8 mL·min^-1,柱温：34 ℃,检测波长：254 nm。结果 芦荟大黄素在9.11～145.76 μg·mL^-1（r=0.999 4）,大黄酸在5.63～90.08 μg·mL^-1（r=0.999 3）,大黄素在5.44～87.04 μg·mL^-1（r=0.999 9）,大黄酚在6.13～98.08 μg·mL^-1(r=0.999 9),大黄素甲醚在2.72～43.52 μg·mL^-1 (r=0.999 8)线性良好;平均回收率分别为97.64%、98.14%、99.52%、99.36%、98.43%;RSD分别为1.29%、1.81%、1.40%、0.59%、1.58%。结论 该方法简便、可靠、准确,可用于疗筋涂膜剂的质量控制。     

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。     

反相高效液相色谱法测定唑克搽剂中盐酸克林霉素的含量

目的建立反相高效液相色谱法测定唑克搽剂中盐酸克林霉素含量的方法。方法色谱柱为Kromail C18柱(4.6 mm×250 mm，5 μm)；柱温：40 ℃；流动相为水-甲醇(21∶30)，含0.02 mol·L^-1磷酸二氢铵和0.01 mol·L^-1乙二胺四醋酸二钠，并以4 mol·L^-1磷酸溶液调节pH值至3.0；流速0.9 mL·min^-1；检测波长为367 nm。结果盐酸克林霉素在10～100 μg·mL^-1的范围内线性关系良好，r＝0.999 6(n＝6)，平均回收率为99.40 %(n＝6)，RSD为1.0 %。结论该方法简便、快速、准确，可用于唑克搽剂的质量控制。     

高效液相色谱法测定依诺沙星制剂中依诺沙星的含量

目的建立依诺沙星制剂中依诺沙星含量的测定方法。方法采用高效液相色谱法（HPLC）法，Kromasil C18色谱柱(200 mm×4.6 mm，7 μm);流动相：0.025 mol·L^-1磷酸（用三乙胺调节pH值至3.0） 甲醇-乙腈（80∶10∶10），流速：1.0 mL·min^-1;检测波长：269 nm;进样量：20 μL。结果依诺沙星主峰与各杂质及降解产物峰能有效分离，在2～20 μg·mL^-1范围内线性关系良好（r＝0.999 8）。依诺沙星片平均回收率100.0%，RSD＝0.8%;依诺沙星胶囊平均回收率98.5%，RSD＝1.2%;依诺沙星滴眼液平均回收率99.1%，RSD＝0.7%;依诺沙星软膏平均回收率98.9%，RSD＝0.9%。结论该方法专属性强，结果准确可靠，可用于各种依诺沙星制剂的含量测定。     

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.