HPLC法测定丝裂霉素C聚氰基丙烯酸正丁酯纳米粒中丝裂霉素C的含量

目的:建立高效液相色谱法测定丝裂霉素 C 聚氰基丙烯酸正丁酯纳米粒(MMC-PBCA-NP)中药物含量。方法:采用C_(18)柱(4.6 mm×150 mm,5 μm),以混合磷酸盐缓冲液-乙腈(85:15)为流动相,流速为1 mL·min~(-1),紫外检测器,检测波长为365 nm。结果:丝裂霉素 C(MMC)浓度在5～250 μg·mL~(-1)范围内与峰面积呈良好的线性关系,r=0.9998;平均回收率(n=6)为98.15%。结论:本法专属性强,操作简便,结果准确。适用于 MMC-PBCA-NP 的质量控制。     

清心牛黄片中芍药苷含量测定方法的探索

目的:建立HPLC法测定清心牛黄片中芍药苷的含量.方法:Symmetry C18色谱柱(150 mm×4.6 mm,5μm);以乙腈-0.1％磷酸水(12∶ 88)为流动相;检测波长为230 nm;柱温30℃;流速1 ml/min.结果:芍药苷在3.3125～53 μg/ml浓度范围内线性关系良好(R2 =0.999 9),回收率为96.18％,RSD为0.42％.结论:建立的含量测定标准可以更有效地控制药品质量.     

用HPLC法同时测定比格犬血浆中地西泮、去甲西泮和氟马西尼的浓度

目的:建立测定比格犬血浆中地西泮、去甲西泮和氟马西尼浓度的HPLC法.方法:采用Kromasil 100-5 C18色谱柱(250 mm×4.6 mm,5μm);以氯硝西泮为内标,甲醇(A)-水(B)-四氢呋喃(C)为流动相(55∶40∶5),流速1.0 ml/min,检测波长254 nm;柱温25 C.结果:地西泮、去甲西泮和氟马西尼在浓度范围为0.025～1.000 μg/ml时线性良好(r=0.999 9,0.999 0,0.998 9),日内和日间RSD均＜6％(n=5),回收率接近100％.结论:本方法准确、快速、简便,可用于比格犬血浆中地西泮、去甲西泮和氟马西尼浓度的同时测定.     

高效液相色谱法同时测定人血浆中帕罗西汀与氯氮平浓度

目的 建立同时测定人血浆中帕罗西汀、氯氮平浓度的高效液相色谱法.方法 以Diamonsil C18反相柱(150 mm×4.6 mm,5.μm)为色谱柱,流动相为30 mmol/L醋酸铵-甲醇(25:75);流速:1.0 mL/min;柱温:40℃;检测波长:265 nm.以乙酸乙酯-二氯甲烷(80:20)为提取剂.结果 帕罗西汀在10.0 ～640.0μg,/L、氯氮平在25.0～1 000.0 μg/L浓度范围内,峰面积与其浓度呈良好线性关系;帕罗西汀、氯氮平的低、中、高3种浓度相对平均回收率大于95％,提取回收率大于70％.日内、日间RSD均低于15％(n=5);分析方法的检测限5.0 μg/L.帕罗西汀线性方程:y=23.325X+2.78,r=0.998 2(n=7);氯氮平线性方程:Y=28.651X+ 1.82,r=0.998 6(n =7).结论 该方法灵敏、准确、简单、快速,可用于临床帕罗西汀与氯氮平血药浓度监测和药动学研究.     

高效液相色谱法测定复方丹参输卵管灌注液中丹参素含量

目的 建立高效液相色谱法测定复方丹参输卵管灌注液中丹参素含量.方法 色谱柱:Inertsil C18柱(4.6 mm × 250 mm,5 μm);流动相:甲醇-1％冰醋酸,梯度洗脱;流速:1.0ml/min;检测波长:280 nm.结果 丹参素检测浓度在8.5～42.5 μg/ml范围内与峰面积呈良好的线性关系(0.999 9);平均加样回收率为98.36％,RSD为1.02％.结论 该方法简单、灵敏、准确,可用于复方丹参输卵管灌注液的质量控制.     

自动柱切换高效液相色谱法同时测定血浆中的SMZ和TMP

应用自制自动柱切换装置建立了同时测定SMZ及TMP血药浓度的HPLC方法.采用μBondapak C 18(50mm×4.6mm.37～50μm)为预处理柱,水为预处理流动相.分析柱为Hypersil BDS C18(150mm×4.6mm,5μm)柱,分析流动相为甲醇:磷酸缓冲液=35:65.检测波长230nm.SMZ和TMP分别在2.5～80μg/ml及0.125～4μg/ml范围内线性良好(r_1=0.999 7,r_2=0.9998).平均方法回收率分别为98.59%及95.71%;日内精密度分别为2.11%及2.67%,日间精密度分别为2.51%及2.89%;两者的最低血浆检测浓度可达SMZO.1μg/ml,TMPO.02μg/ml.方法迅速、简便、灵敏.     

HPLC法测定阿法替尼片中主药和有关物质的含量

目的:建立以高效液相色谱法测定阿法替尼片中主药和有关物质含量的方法,以控制该制剂的质量.方法:色谱柱为Kromasil C18(250 mm×4.6 mm,5μm),流动相为乙酸铵水溶液(30 mmol/L)-甲醇(25∶ 75),流速为1.0ml/min,紫外检测波长为254 nm,柱温30℃,进样量为20 μl.结果:阿法替尼检测浓度的线性范围为60.13～600.45μg/ml(r =0.999 6);平均回收率为99.41％,RSD为0.86％.结论:建立的检测方法简单,结果准确可靠,可用于阿法替尼片的质量控制.     

柱前衍生RP-HPLC法测定丙戊酸钠的血药浓度及监测结果分析

目的:建立柱前衍生RP-HPLC法测定人血浆中丙戊酸钠血药浓度并对监测结果进行分析.方法:环己烷羧酸为内标,2-溴-对硝基苯乙酮为衍生化试剂,Hypersil BDS C18柱(4.6 mm×200 mm,5 μm)为分析柱;甲醇-水(79:21)为流动相,检测波长为265 nm,流速1.0 mL/min,柱温30℃,用柱前衍生RP-HPLC法对10 066例次癫痫患儿进行丙戊酸钠血药浓度测定.结果:内标环己烷羧酸和丙戊酸钠衍生物的保留时间分别为6.2 min、8.1 min,丙戊酸钠浓度在13.6～326.4 μg/mL范围内样品浓度与峰面积比之间线性关系良好(r=0.9989),最小可定量浓度为13.6 μg/mL,平均方法回收率为95.0％～105.0％,日内日间RSD均＜10％.10066例次癫痫惠儿血药浓度监测结果在治疗浓度(50～100μg/mL)内的共5 100例次,占50.7％;低于治疗浓度范围下限(＜50 μg/mL)共4 313例次,占42.8％;高于治疗浓度范围上限(＞100 μg/mL)的共653例次,占6.5％.结论:本测定方法简便快捷,灵敏准确,可用于临床丙戊酸钠血药浓度的监测;癫痫患儿应用丙戊酸钠个体差异较大,应监测其血药浓度,实施个体化给药.     

高效液相色谱法测定参芪几丁聚糖胶囊中特女贞苷含量

目的:建立参芪几丁聚糖胶囊中特女贞苷含量测定的方法.方法:采用高效液相色谱法,色谱柱为Waters Symmetry C18柱(250 mm×4.6 mm,5μm),甲醇-水(40:60)为流动相,检测波长224 nm,柱温35℃,流速为1.0 ml/min,进样量为10μl.结果:特女贞苷浓度在2.5～125μg/m...     

简单灵敏的HPLC法测定人血浆中头孢丙烯浓度

目的:建立血浆中头孢丙烯的HPLC检测方法.方法:采用高效液相色谱检测法,分析柱为Hypersil BDS C18 (200 mm×4.6 mm,5μm),流动相为20 mmol/L乙酸铵/10％乙酸(pH=3.7):乙腈=92:8(V/V),流速1.0 mL/min,柱温30℃,检测波长282 nm,进样量20μL.血浆样品用三氟醋酸直接沉淀后,取上清进样分析.结果:头孢丙烯在0.10～10.01 μg/mL范围内线性关系良好(r=1.0000),最低定量浓度为0.10μg/mL,日内日间RSD均＜15％(n=15).结论:研究建立的HPLC法快速、简便、高效,精密度和准确度高,适合血样中头孢丙烯浓度的检测.     

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.