HPLC法测定链麻滴鼻液中硫酸链霉素和盐酸麻黄碱的含量

目的建立测定链麻滴鼻液中硫酸链霉素和盐酸麻黄碱含量的高效液相色谱法,消除焦亚硫酸钠对硫酸链霉素含量测定的影响。方法色谱柱为Diamonsil C18柱(250mm×4.6mm,5μm);流动相为0.014mol·L-1庚烷磺酸钠的0.05mol·L-1磷酸二氢钾溶液-乙腈(78∶22);检测波长硫酸链霉素195nm,盐酸麻黄碱207nm;流速1.0mL·min-1。结果硫酸链霉素质量浓度在44.40³10.80μg·mL-1范围内,与其峰面积呈良好的线性关系。(r=0.999 8,n=7),平均回收率为103.4%(RSD=3.4%);盐酸麻黄碱质量浓度在20.224310.80μg·mL-1范围内,与其峰面积呈良好的线性关系。(r=0.999 8,n=7),平均回收率为103.4%(RSD=3.4%);盐酸麻黄碱质量浓度在20.224⁸0.896μg·mL-1范围内,与其峰面积呈良好的线性关系(r=0.999 9,n=7),平均回收率为99.5%(RSD=1.0%)。结论该方法专属性强、测定结果准确、精密度高、线性好,加入甲醛能够消除辅料中焦亚硫酸钠对硫酸链霉素含量测定的影响。     

呋麻滴鼻液的质量标准研究

目的建立呋麻滴鼻液的质量标准。方法用高效液相色谱法对呋麻滴鼻液中盐酸麻黄碱和呋喃西林进行鉴别和含量测定,采用Phenomenex C18色谱柱,以0.1 mol·L-1醋酸铵(用冰醋酸调节pH3.0)-乙腈(85∶15)为流动相,检测波长为254 nm,柱温为室温。结果高效液相色谱法检测出盐酸麻黄碱和呋喃西林。盐酸麻黄碱在156.25～1 250.00μg·mL-1范围内线性关系良好,r=0.999 8,平均回收率为97.21%(n=5),RSD为0.9%;呋喃西林在3.12～25.00μg·mL-1范围内线性关系良好,r=0.999 8;平均回收率为97.21%(n=5),RSD为1.0%。结论该方法简便、快速、准确并且专属性强。     

高效液相色谱法测定麻氟滴鼻液中两组分的含量

目的建立测定麻氟滴鼻液中盐酸麻黄碱和地塞米松磷酸钠含量的方法。方法采用高效液相色谱（HPLC）法，色谱柱为Hypersil BDS C18柱（250mm×4．6mm，5μm），流动相为0.025mol／L磷酸二氢钾（加入0．5％三乙胺，用磷酸调节pH值至3．5）-甲醇-乙腈（52：38．4：9．6），流速为0．9mL／min，检测波长为257nm，柱温为40℃。结果盐酸麻黄碱质量浓度在100～600μg／mL范围内与峰面积线性关系良好（r=0．9998），平均回收率为100．54％，RSD=1．0％（n=6）；地塞米松磷酸钠质量浓度在10～60μg／mL范围内与峰面积线性关系良好（r=0．9998），平均回收率为100．20％，RSD=1．2％（n=6）。结论HPLC法专属性好，操作简便、快速，结果准确，可用于麻氟滴鼻液的质量控制。     

HPLC法测定麻地滴鼻液中两组分含量

目的建立HPLC法测定麻地滴鼻液中盐酸麻黄碱和地塞米松磷酸钠的含量。方法采用Hypersil ODS2(4.6 mm×250mm,5μm)色谱柱,以甲醇∶0.025 mol.L-1磷酸二氢钠溶液(54∶46)为流动相,流速1.0 m l.m in-1,检测波长258 nm。结果盐酸麻黄碱和地塞米松磷酸钠的线性范围分别为102~510 mg.L-1,(r=0.999 9),2.5~12.5 mg.L-1,(r=1.0);平均加样回收率分别为100.9%(RSD=1.1%),101.1%(RSD=1.5%)。结论该方法简便、准确,适用于麻地滴鼻液的质量控制。     

RP-HPLC测定复方麻黄碱滴鼻液中盐酸麻黄碱、盐酸林可霉素和地塞米松磷酸钠含量的方法学研究

目的 建立反相高效液相色谱法测定复方麻黄碱滴鼻液中盐酸麻黄碱、盐酸林可霉素和地塞米松磷酸钠含量的方法.方法采用Dikma C18(150 mm x4.6 mm,5μm)色谱柱,甲醇-0.05mol·L-1硼砂缓冲液(用磷酸调节pH值至6.0)(4753)为流动相,检测波长为241nm.结果盐酸麻黄碱、盐酸林可霉素、羟苯乙酯(尼泊金乙酯)和地塞米松磷酸钠的分离度完全达到要求.盐酸麻黄碱浓度在2.55～30.63 mg·mL-1内线性关系良好(r=0.999 9);盐酸林可霉素在2.58～30.98 mg·mL-1内线性关系良好(r=0.999 6);地塞米松磷酸钠在49.53～594.30 μg·mL-1内线性关系良好(r=1.000 0);平均回收率分别为99.75%(RSD为0.77%)、102.11%(RSD为0.94%)、99.69%(RSD为0.72%).结论 本方法准确、专属、简便、快速,能有效地控制产品的质量.     

HPLC法同时测定扑麻滴鼻液中2成分的含量

目的:建立同时测定扑麻滴鼻液中盐酸麻黄碱和马来酸氯苯那敏含量的HPLC方法。方法:采用:PurospherSTAR RP18色谱柱(150 mm×4.6 mm,5μm),以磷酸盐缓冲液(p H 3.0±0.1)-乙腈(82∶18)为流动相,流速为1.0 ml·min-1,在210nm波长处同时检测盐酸麻黄碱和马来酸氯苯那敏,柱温35℃,进样量20μl。结果:盐酸麻黄碱和马来酸氯苯那敏分别在19.81~118.85μg·ml-1和6.21~37.25μg·ml-1浓度范围内线性关系良好,r分别为0.999 6和0.999 8。平均回收率分别为100.39%(RSD=0.69%,n=9)和100.11%(RSD=0.60%,n=9)。结论:该方法快速简便、重复性、准确性好,可用于该制剂中盐酸麻黄碱和马来酸氯苯那敏的含量测定。     

磺胺嘧啶麻黄碱滴鼻液定性定量方法研究

目的研究磺胺嘧啶麻黄碱滴鼻液的定性定量方法。方法采用化学反应法及HPLC法定性定量鉴别处方中的磺胺嘧啶及盐酸麻黄碱。采用HPLC法测定磺胺嘧啶及盐酸麻黄碱的含量,色谱柱为Hibar RP-18endcapped(150 mm×4.6 mm,5μm),流动相为磷酸盐缓冲液(p H值为3.0±0.1)-乙腈(90∶10),流速1.0m L?min-1,检测波长210 nm。结果化学反应和HPLC法均能定性鉴别磺胺嘧啶及盐酸麻黄碱。磺胺嘧啶和盐酸麻黄碱分离良好;进样浓度分别为99.96²99.88μg?m L-1(r=0.999 8,n=5)和19.86299.88μg?m L-1(r=0.999 8,n=5)和19.86⁵9.58μg?m L-1(r=0.999 9,n=5)与峰面积呈良好的线性关系。磺胺嘧啶和盐酸麻黄碱的平均回收率在98.0%59.58μg?m L-1(r=0.999 9,n=5)与峰面积呈良好的线性关系。磺胺嘧啶和盐酸麻黄碱的平均回收率在98.0%¹00%,RSD均<1.2%(n=3)。结论本方法简便、快速、准确,重复性好,可用于磺胺嘧啶麻黄碱滴鼻液的质量控制。     

HPLC法测定氯麻滴鼻液中氯霉素和盐酸麻黄碱的含量

目的 建立测定氯麻滴鼻液中氯霉素和盐酸麻黄碱含量的高效液相色谱法.方法 采用Waters C18色谱柱（4.6mm×250 mm,5μm）,流动相为0.01 mol·L-1磷酸二氢钾溶液（用磷酸和三乙胺调节pH=3.0）-乙腈（60∶40）,流速为1.0 mL· min-1,检测波长为220 nm,柱温为30℃.结果 氯霉素在9.84～98.45 μg·mL-1范围内线性关系良好,盐酸麻黄碱在40.24～402.39 μg·mL-1范围内线性关系良好.氯霉素平均回收率为100.89％,RSD=0.21％;盐酸麻黄碱平均回收率为100.33％,RSD=0.83％.结论 本方法灵敏度高、操作简便、准确可靠,可用于氯麻滴鼻液中氯霉素和盐酸麻黄碱的含量测定.     

新麻滴鼻液中盐酸麻黄碱与硫酸新霉素的含量测定

目的:建立新麻滴鼻液中盐酸麻黄碱和硫酸新霉素的含量测定方法.方法:用高效液相色谱法测定样品中盐酸麻黄碱的含量;用分光光度法测定样品中硫酸新霉素的含量.结果:盐酸麻黄碱在0.05～1.50 g·L-1范围内线性关系良好,r=0.999 8,平均回收率为101.28%(RSD≤1.16%);硫酸新霉素在60～420 IU·mL-1范围内线性关系较好,r=0.999 0,平均回收率为102.19%(RSD≤2.74%).结论:所建立的测定方法准确、重复性好、实用.     

HPLC法测定鼻炎糖浆中盐酸麻黄碱和盐酸伪麻黄碱的含量

目的建立高效液相色谱法测定鼻炎糖浆中盐酸麻黄碱和盐酸伪麻黄碱含量的测定方法。方法采用Agilent Zorbax SB-C18色谱柱(4.6 mm×250 mm,5μm),乙腈-0.2%磷酸溶液(含0.2%三乙胺)(2∶98)为流动相,流速:1.0 m L·min-1,检测波长206 nm,柱温:25℃。结果盐酸麻黄碱进样量在0.124¹.86μg范围内与峰面积呈良好线性(r=0.999 9),平均回收率为99.99%,RSD=1.24%(n=6);盐酸伪麻黄碱进样量在0.103 81.86μg范围内与峰面积呈良好线性(r=0.999 9),平均回收率为99.99%,RSD=1.24%(n=6);盐酸伪麻黄碱进样量在0.103 8¹.557μg范围内与峰面积呈良好线性(r=0.999 9),平均回收率为99.33%,RSD=1.93%(n=6)。结论该方法准确、重复性好,可用于鼻炎糖浆中盐酸麻黄碱和盐酸伪麻黄碱的测定。     

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.