HPLC法测定抗炎退热片中黄芩苷的含量

目的：建立高效液相色谱法测定抗炎退热片中黄芩苷的含量。方法：采用高效液相色谱（HPLC）法，以C18柱（250nma×4．6mm；φ5μm）为色谱柱；以甲醇-0．1％磷酸溶液（50：50）为流动相；检测波长为280nm；流速为1．0ml／min。结果：黄芩苷进样量在6-296μg／ml范围内与峰面积线性关系良好（r=0．9999），平均回收率为99．35％，RSD=0．794％（n=6）。结论：HPLC法，决速、准确、重现性好，可用于抗炎退热片的质量控制。     

HPLC法与UPLC法同时测定黄芩中5种黄酮类成分含量的比较

目的:为黄芩多指标成分同步质量控制提供更加简便、快捷的检测方法。方法:分别采用高效液相色谱(HPLC)法和超高效液相色谱(UPLC)法测定黄芩中黄芩苷、汉黄芩苷、黄芩素、汉黄芩素和千层纸素A含量,比较两种方法的分离情况、线性关系、精密度、重复性、稳定性和加样回收率。HPLC法色谱柱为Diamonsil C18(250 mm×4.6 mm,5μm),流动相为乙腈-水-甲酸(梯度洗脱),柱温为30℃,流速为1.0 ml/min,检测波长为280 nm;UPLC法色谱柱为Aquity BEH C18(50 mm×2.1 mm,1.7μm),流动相为0.1%甲酸水溶液-乙腈(梯度洗脱),柱温为40℃,流速为0.4 ml/min,检测波长为280 nm。结果:两种方法在各自对应条件下的分离情况良好;进样量与峰面积积分值均呈良好的线性关系(r≥0.999 5);精密度、稳定性和重复性试验RSD<4%;平均加样回收率均>96%(RSD<5%,n=6);样品测定结果差异无统计学意义(P>0.05)。结论:UPLC法较HPLC法具有速度更快、灵敏度更高,且节省溶剂的优势。UPLC法可以成功代替HPLC法,应用于黄芩药材多指标成分的同步质量控制。     

滴通鼻炎水中黄芩苷含量的测定

目的 建立高效液相色谱法(HPLC法)测定滴通鼻炎水中黄芩苷含量的方法.方法 采用C18250 mm×4.6 mm色谱柱,以甲醇-0.2%磷酸溶液(5149)为流动相,流速1.0 ml/min,检测波长为280 nm.结果 黄芩苷进样量在8.4～42μg范围内,线性关系良好,r=0.9999;平均回收率为99.11%,RSD为1.5%.结论 本法测定黄芩苷含量简便、快捷、准确,可用于该制剂的含量测定.     

双花解毒合剂中黄芩苷的质量浓度测定

目的:建立双花解毒合剂中黄芩苷高效液相色谱(HPLC)测定方法。方法:采用高效液相色谱法,色谱柱Kromasil C18(250mm×4.60mm,5μm);以甲醇-0.4%磷酸水(52∶48)为流动相,流速为1mL/min,检测波长为280nm。结果:黄芩苷的线性范围为0.056～0.556μg/mL,r=0.9999,平均加样回收率(n=6)为101.40%,RSD为2.40%。结论:本法简便可行、重复性好,可用于双花解毒合剂中黄芩有效成分的含质量测定。     

高效液相色谱法测定肺炎四号合剂中黄芩苷的含量

目的:建立肺炎四号合剂的含量测定方法.方法:采用高效液相色谱法(HPLC法)测定,色谱柱为Kromasil 0DS C18柱(250 mm×4.6 mm,5 μm),流动相为甲醇-水-冰醋酸(50:50:1),检测波长为274 nm.结果:黄芩苷线性范围是0.097 68～0.488 4μg/mL,r=0.999 8(n=5),加样回收率为98.93%,RSD为0.77%(n=5).结论:HPLC法简便、快速、准确,可作为该制剂的质量控制方法.     

高效液相色谱法测定复方清音饮中绿原酸的含量

目的:建立复方清音饮的质量标准.方法:采用高效液相色谱(HPLC)法,色谱柱:scienhome C 18(250 mm×4.6 mm,5μm);流动相:乙腈-0.4%磷酸(13:87);流速:1.0 ml/min;检测波长:326 nm;柱温:25℃;进样量:20μl.结果:绿原酸在35.2~176μg/ml浓度范围内与峰面积线性关系良好,Y=3.85 E-8 X(r=0.9999),加样回收率为98.6%(n=6),RSD为1.7%.结论:该方法稳定、结果可靠、重复性好,可以有效控制复方清音饮质量.     

高效液相色谱法测定清肺抑火片中黄芩苷的含量

目的:探讨清肺抑火片的含量测定方法.方法:采用高效液相色谱法(HPLC法)测定清肺抑火片黄芩中黄芩苷的含量.色谱柱为Elite 0DS C18柱(250 mm×4.0 mm,5μm),流动相为甲醇-水-磷酸(45:55:0.2),流速为1 mL/min,检测波长为315 nm.结果:回归方程为Y=85.915 4 2 701.674 3X,r=0.999 3,平均回收率为97.93%,RSD为1.76%(n=6).结论:HPLC法简便、快速、可靠,可用于清肺抑火片的质量控制.     

注射用复方荭草冻干粉针中野黄芩苷的含量测定

目的:建立注射用复方荭草冻干粉针中野黄芩苷的定量测定方法.方法:采用高效液相色谱法(HPLC法),以C18柱(250mm×4.6mm,5μm)为色谱柱,以乙腈-0.1%磷酸(18:82)为流动相,检测波长为335 nm.结果:野黄芩苷与其他组分峰的分离度均大于1.5,线性范围为0.15～2.4μg,r=0.999 9,平均回收率为99.89%,RSD为1.22%.结论:HPLC法简便、准确、重现性好,适用于该制剂的质量控制.     

高效液相色谱法测定清喉咽合剂中黄芩苷的含量

目的:建立一种用高效液相色谱法测定清喉咽合剂中黄芩苷含量的方法。方法:高效液相色谱法,色谱柱 YMC—Pack 0DS—A C18 150×4.6mm I.D.S—5μm,12nm;流动相为甲醇—水—磷酸(50:50:0.3);检测波长:278nm;流速1ml/min。结果:黄芩苷在10～60μg/ml 浓度范围内与峰面积呈良好的线性关系(r=0.9996)。精密度为0.06%。平均回收率为99.26%。结论:该方法快速,准确,专属性好,灵敏度高。     

复方地黄合剂及复方逍遥合剂中黄芩苷含量测定

目的 :建立复方地黄合剂及复方逍遥合剂中黄芩苷含量的测定方法.方法 :采用高效液相色谱(HPLC)法、C18色谱柱(4.6 mm×250 mm,5μm)、流速1.2 ml/min,柱温25℃,波长280 nm测定,流动相为乙腈-0.2%磷酸溶液(27:73).结果 :在不同中药制剂中,黄芩苷峰形良好,方法专属性强.在浓度为16~320μg/ml范围内均呈良好的线性关系(r=0.9993);在50%、100%、150%的浓度下,二制剂中黄芩苷的回收率分别为99%及97%,RSD分别为1.7%和1.6%.此外,黄芩苷在8 h内含量变化的RSD分别为0.3%和0.2%,稳定性良好.结论 :该方法简便、准确、灵敏度高、重复性好,可用于复方地黄合剂及复方逍遥合剂中黄芩苷的含量的测定.     

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.