HPLC法测定维生素B2片的含量及有关物质

目的建立高效液相色谱法测定维生素B2片的含量和有关物质。方法采用C18色谱柱(250 mm×4.6 mm,5μm);以甲醇—乙腈—10 mmol.L-1庚烷磺酸钠溶液(含冰醋酸为0.5%)(5∶10∶85)为流动相;检测波长:444 nm;流速:1.0 mL.min-1。结果在建立的色谱条件下,维生素B2能与杂质完全分离;维生素B2在0.111 7～0.893 8μg范围内线性关系良好,r=1.000;平均回收率为100.5%(n=9);测定维生素B2的最小检出量为2.2 ng。结论该方法操作方便、准确,灵敏度高,专属性强,可用于维生素B2片的质量控制。     

用HPLC法测定参维冻干蜂王浆片中维生素B1和维生素B2含量

目的 建立参维冻干蜂王浆片中维生素B1和维生素B2的含量测定方法.方法 用KANTO CHEMICAL Co.,Inc,Mightysil C18色谱柱(250×4.6 mm,5μm),以乙腈-0.032%的辛烷基磺酸钠溶液(取辛烷基磺酸钠0.32g,加冰醋酸3ml和三乙胺3ml,加水溶解至1000ml)(10∶90)为流动相,流速1.0ml·min-1,检测波长为270nm,柱温为35℃.结果 维生素B1的线性范围为16μg·ml-1～800μg·ml-1(r=0.9999),平均回收率为99.4%,RSD=0.9%(n=9);维生素B2的线性范围为2μg·ml-1～104μg·ml-1(r=1.0000),平均回收率为99.6%,RSD=0.7%(n=9).结论 HPLC法适用于参维冻干蜂王浆片中维生素B1和维生素B2的含量测定.     

五维甘草那敏胶囊中泛酸钙、维生素B2含量测定方法改进

目的利用高效液相色谱法同时测定五维甘草那敏胶囊中泛酸钙、维生素B₂的含量。方法色谱柱:Agilent Eclipse Plus C18(4.6 mm×250 mm,5μm);流动相:甲醇-0.5%磷酸溶液(28∶72);进样量:10μL;柱温为30℃;流速:1.0 m L·min^-1;检测波长为210 nm。结果泛酸钙、维生素B2分别在40.76~815.2,10.56~211.2μg·m L^-1范围内线性关系良好。回归方程分别为:Y₁=3.3×10³X+1.4×10⁴(r=0.999 5,n=6),Y₂=1.9×10⁴X-1.9×10³(r=0.999 4,n=6);平均回收率分别为98.82%(RSD=0.76%)、98.54%(RSD=0.98%)。精密度分别为0.63%、0.88%(n=6)。结论该方法经方法学验证,可用于五维甘草那敏胶囊中泛酸钙、维生素B2的含量测定。     

高效液相色谱法同时测定复方壬二酸乳膏中维生素C与维生素E的含量

目的:建立高效液相色谱外标法同时测定复方壬二酸乳膏中维生素C与维生素E的含量的方法。方法:色谱柱为Hypersil ODS2(5.0mm×250mm,5μm);流动相为甲醇-水-磷酸(98∶2∶0.4),流速为1.0mL.min-1,柱温为室温,检测波长为285nm。结果:维生素C在128.6~422mg.L-1范围内呈良好线性关系,A1=52709.95C1-3969.33,r=0.9991(n=5);维生素E在124.5~415mg.L-1范围内呈良好线性关系,A2=11254.57C2 14453.15,r=0.9999(n=5);维生素E平均回收率为99.50%;维生素C的平均回收率为99.29%;RSD分别为0.85%和0.74%。结论:该方法操作简便,结果准确,重复性好。     

HPLC法测定维生素B1片含量均匀度

目的建立高效液相色谱法测定维生素B1片含量均匀度。方法采用色谱柱:Diamonsil C18(150mm×4.6mm,5μm),以碳十八烷基键合硅胶为填充剂。流动相:甲醇-乙腈-0.02mol/L庚烷磺酸钠溶液(含1%三乙胺,用磷酸调节pH值至5.5,9∶9∶82);检测波长为238nm,流速为1.0ml/min;进样量:10μl。结果维生素B1质量浓度在50.5~505μg/ml范围内与峰面积呈良好的线性关系(r=0.99999,n=5),平均回收率为100.4%,RSD=0.13%。结论本方法简单、精确、可靠,可作为维生素B1片的质量控制方法。     

HPLC法测定维生素B_1注射液含量

目的建立维生素B1注射液含量测定HPLC方法。方法色谱柱：Spherisorb C18（4.6mm×200mm,5μm）,流动相：乙腈-0.008mol.L^-1己烷磺酸钠-三乙胺-冰醋酸（12∶87∶0.27∶0.73）,流速1.0mL.min^-1,检测波长为246nm。结果维生素B1在0.083-0.414μg进样量范围内线性关系良好（r=0.9999）;平均回收率分别为：维生素B199.03%（RSD为0.41%）。结论本法快速、灵敏、准确,重现性好,可作为维生素B1注射液的含量测定方法。     

反相高效液相色谱法测定甲硫氨酸维生素B1注射液的含量及其有关物质

目的:建立一种离子对反相高效液相色谱法测定甲硫氨酸维生素 B_1注射液中甲硫氨酸、维生素 B_1两组分的含量及其有关物质。方法:采用 Lichrospher C_(18)(4.6 mm×250 mm,5μm)色谱柱,水相(己烷磺酸钠0.216 g,加水500 mL 溶解后,加三乙胺2 mL,用磷酸调 pH 至3.1)-甲醇(94:6)为流动相,流速1 mL·min~(-1),检测波长210 nm,进样量20μL,外标法定量。结果:甲硫氨酸和维生素 B_1线性范围分别为20～200μg·mL~(-1)(r=0.9999)和2～20μg·mL~(-1)(r=0.9995);两组分的定量限分别为100 ng·mL~(-1),33 ng·mL~(-1);最低检测限约为30 ng·mL~(-1),10 ng·mL~(-1)。测得低、中、高3个浓度,两组分的平均回收率分别在为100.2%～101.5%(RSD≤1.4)和99.0%～99.8%(RSD≤0.75)之间。结论:本方法简便、快速、准确,专属性好,可用于甲硫氨酸维生素 B_1注射液中两组分的含量及其有关物质的测定。     

HPLC法同时测定更年安软胶囊中维生素B_1、维生素B_6的含量

目的:建立用反相高效液相色谱法同时测定更年安软胶囊中维生素B1、维生素B6含量的方法。方法:采用C18(250 mm×4.6 mm,5μm)色谱柱,流动相为甲醇-0.06%庚烷磺酸钠溶液(含1.2%醋酸与0.12%三乙胺)25∶75,检测波长275 nm,流速0.8 mL·min-1。结果:维生素B1和维生素B6线性范围分别为16.02～80.10μg·mL-1和15.84～79.20μg·mL-1,相关系数r分别为0.9996和0.9997;平均回收率分别为101.2%(RSD=0.5%)和100.1%(RSD=0.9%)。结论:该法可同时测定更年安软胶囊中维生素B1、维生素B6的含量,方法简便、准确,重复性好。可为制定更年安软胶囊的质量标准和产品质量控制提供依据。     

精蛋白锌胰岛素注射液中硫酸鱼精蛋白含量测定的方法研究

目的:建立高效液相色谱(HPLC)法测定精蛋白锌胰岛素注射液中硫酸鱼精蛋白的含量。方法:采用Grace Vydac C18色谱柱(250 mm×4.6 mm,5μm),以A:乙腈-0.2 mol.L-1硫酸钠溶液(4∶96);B:乙腈-水(50∶50)为流动相进行梯度洗脱(0～8 min时B0%→70%,8～15 min时B70%,15～16 min时B70%→0%,16～30 min时B0%);流速1.0 mL.min-1;柱温40℃;检测波长:214 nm。结果:硫酸鱼精蛋白线性范围为0.05～2.5 mg.mL-1(r=0.9994),方法平均回收率(n=9)为99.7%。结论:本方法准确、简便、快速,重复性好,可用于精蛋白锌胰岛素注射液中硫酸鱼精蛋白的含量测定。     

高效液相色谱 荧光检测法测定维酶素片中维生素B2的含量

目的：建立高效液相-荧光检测法测定维酶素片中维生素B2含量的方法。方法：色谱柱为PAKC18柱（250 mm×4.6 mm,5μm）,流动相为甲醇-0.02 mol·L-1乙酸铵（35∶65）,流速：1.0 ml·min-1,进样量：10μl,柱温：25℃。荧光检测激发光波长：450 nm,发射光波长：522 nm。结果：维生素B2的含量在1.0~20.0μg·m1-1之间线性关系良好（r=0.999 9）,平均回收率为99.20%,（RSD=0.63%,n=6）。结论：此方法专属性强、灵敏度高、结果准确,可用于该片剂中维生素B2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.     

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.     

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.