HPLC法同时测定防风通圣颗粒中6种成分的含量

摘要：目的:建立采用HPLC法同时测定防风通圣颗粒中盐酸麻黄碱、盐酸伪麻黄碱、栀子苷、黄芩苷、汉黄芩苷、甘草酸含量的方法。方法:采用Welch Ultimate Phenyl-Ether色谱柱（250 mm×4.6 mm,5μm）;流动相为乙腈-0.2%磷酸（含0.1%NH4Cl）,梯度洗脱;流速为1.0 ml·min-1;柱温为30℃;检测波长分别为210 nm（盐酸麻黄碱、盐酸伪麻黄碱）、238 nm（栀子苷）、278 nm（黄芩苷、汉黄芩苷）、252 nm（甘草酸）;进样量10μl。结果:盐酸麻黄碱、盐酸伪麻黄碱、栀子苷、黄芩苷、汉黄芩苷、甘草酸分别在2.07～20.67μg·ml-1（r=0.999 6）、1.14～11.37μg·ml-1（r=0.999 4）、3.13～31.33μg·ml-1（r=0.999 7）、20.73～207.30μg·ml-1（r=0.999 9）、4.95～49.55μg·ml-1（r=0.999 8）、7.98～79.76μg·ml-1（r=0.999 9）范围内呈良好的线性关系;6种成分加样回收率的平均值分别为98.79%、98.12%、99.24%、102.26%、96.66%、100.57%,RSD分别为2.42%、2.12%、2.47%、2.36%、2.34%、1.93%（n=6）。结论:所建立的方法准确、重复性好,可用于防风通圣颗粒中6种成分的同时测定,并为质量控制体系的完善提供依据。     

HPLC法同时测定复方诺氟沙星滴鼻液中的诺氟沙星和盐酸麻黄碱

目的　建立一种快速、准确的高效液相色谱法同时测定诺氟沙星 ( NOR)和盐酸麻黄碱 ( EPH)的含量。 方法　使用 C1 8色谱柱 ,流动相为乙腈— 0 .1%磷酸 ( 15 :85 V/V) ,检测波长为 2 5 6nm。结果 　样品测定在 9min内完成。诺氟沙星在 10～ 60μg· ml- 1 浓度范围内 ,r=0 .9999,RSD= 0 .46% ,平均回收率为 99.91% ;盐酸麻黄碱在 2 5～ 12 5 μg· ml- 1浓度范围内 ,r=0 .9992 ,RSD=0 .5 1% ,平均回收率为 10 0 .0 3%。 结论 　方法可快速准确地检测复方诺氟沙星滴鼻液中的诺氟沙星和盐酸麻黄碱含量     

高效液相色谱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 :采用反相 μ Bondpak色谱柱 ,甲醇- 0 .0 2mol·L-1磷酸二氢钾 (5 5∶45 ,磷酸调 pH值3.5 )为流动相 ,检测波长 2 5 4nm。结果 :氯霉素和盐酸麻黄碱的线性范围分别为 2 0～ 12 0 μg·ml-1(r =0 .9998) ,80～ 480 μg·ml-1(r =0 .9998) ;加样回收率分别为 10 1.4% ,RSD =0 .5 %及 10 0 .8% ,RSD =0 .9% (n =5 ) ,日内RSD分别为 0 .9%和 0 .4% (n =5 ) ,日间RSD分别为 1.0 %和 0 .8% (n =4)。结论 :HPLC法可用于本制剂的含量测定和质量控制 ,方法简便、灵敏、结果准确     

固相萃取高效液相法测定复方川贝精胶囊中3种麻黄碱成分的含量

摘要：目的:建立同时测定复方川贝精胶囊中盐酸麻黄碱、盐酸伪麻黄碱和盐酸甲基麻黄碱含量的方法。方法:采用固相萃取高效液相色谱法,色谱柱为Phenomenex Luna C18（2）柱（150 mm×4.60 mm,5μm）,流动相为乙腈-0.1%磷酸溶液（2∶98）,检测波长为210 nm,流速为1.0 ml·min-1,柱温为25℃。结果:盐酸麻黄碱、盐酸伪麻黄碱和盐酸甲基麻黄碱的浓度分别在2.0～128.0,0.8～51.2,0.4～9.0μg·ml-1范围内与各自色谱峰面积呈良好线性关系（r=1.000 0）;盐酸麻黄碱、盐酸伪麻黄碱和盐酸甲基麻黄碱的平均加样回收率分别为98.90%（RSD=0.51%）、98.49%（RSD=0.87%）、97.50%（RSD=1.15%）（n=6）。结论:该方法简便、快速、准确,专属性、重复性良好,可用于复方川贝精胶囊的质量控制。     

高效液相色谱法测定复方茶碱麻黄碱片的含量

建立高效液相色谱法测定复方茶碱麻黄碱片中可可碱、茶碱、盐酸麻黄碱及咖啡因的含量测定方法.采用Kromasil C18色谱柱;流动相0.05mol·L-1磷酸二氢钾溶液-甲醇-三乙胺(72280.2);检测波长215nm;流速1.0ml·min-1;柱温42℃.线性范围可可碱为5～125μg·ml-1(r=0.9999,n=6),茶碱为5～125μg·ml-1(r=0.9999,n=6),盐酸麻黄碱2～50μg·ml-1(r=0.9996,n=6),咖啡因3～75μg·ml-1(r=0.9999,n=6);平均回收率(X±SD)分别为可可碱(99.9±0.19)%,茶碱(99.9±0.26)%,盐酸麻黄碱(99.6±0.33)%,咖啡因(99.8±0.23)%.本方法简便、准确、重现性好,适用于复方茶碱麻黄碱片的质量控制.     

混合取代基—β—环糊精—毛细管电泳法分离测定麻黄碱和伪麻黄碱

目的:建立毛细管电泳法同时分离测定同分异构的2对手性化合物麻黄碱和伪麻黄碱的含量。方法:Waters CapillaryIon Analyzer,50μm×60cm空心熔融石英毛细管柱,柱上紫外检测。电泳条件:分离用缓冲液为25mmol·L~(-1)的磷酸-Tris 缓冲液,含18mmol·L~(-1)的羧甲基-β-环糊精和7.5mmol·L~(-1)的β-环糊精-硫酸酯,pH3.02。分离电压:18kV;温度:25℃;虹吸进样,高度10cm,时间1s;紫外检测波长214nm。结果:左旋伪麻黄碱、右旋麻黄碱、左旋麻黄碱和右旋伪麻黄碱线性范围分别为23.7～237μg·ml~(-1),25.0～250μg·mL~(-1),25.0～250μg·mL~(-1),25.4～254μg·mL~(-1),以信噪比等于3:1为标准,最小检测浓度均为5.0μg·mL~(-1);日内和日间精密度RSD在2.4％～4.3％之间。结论:方法分离效率高、简便、快速、成本低。     

毛细管区带电泳法快速测定人血清中氯氮平含量

目的 :建立用毛细管区带电泳快速测定血清中氯氮平含量的方法。方法 :采用 33.5mmol·L-1磷酸盐缓冲液 (pH6 .47) ,用紫外检测器在 2 5 4nm波长处检测 ,以外标法定量。结果 :线性范围 0 .1～ 10 μg·ml-1,最低检测限 0 .1μg·ml-1。平均回收率 ( 97.47± 2 .8) %。日内与日间RSD分别为 2 .6 3%和 3.81%。结论 :毛细血管带电泳法是快速测定人血清中氯氮平含量的较好方法。     

超高效液相色谱法测定风湿骨痛丸中5种成分的含量

目的： 采用超高效液相色谱法（UPLC）测定风湿骨痛丸中乌头碱、次乌头碱、新乌头碱、麻黄碱、伪麻黄碱5种成分的含量。方法： （1）乌头碱、次乌头碱、新乌头碱检测方法：色谱柱为ACQUITY UPLC HSS T3柱（100 mm×2.1 mm,1.8 μm）,ACQUITY UPLC HSS T3预柱（5 mm×2.1 mm,1.8 μm）,流动相为甲醇-0.3 mol·L^-1三乙胺（65∶35,V/V）,流速0.3 mL·min^-1,柱温30℃,检测波长235 nm,进样量10 μL;（2）麻黄碱、伪麻黄碱检测方法：色谱柱为ACQUITY UPLC BEH C₁₈柱（100 mm×2.1 mm,1.7 μm）,流动相为乙腈（A）-0.1%磷酸溶液（B）,采用梯度洗脱,流速0.3 mL·min^-1,柱温30℃,检测波长210 nm,进样量10 μL。结果： 乌头碱、次乌头碱、新乌头碱、麻黄碱、伪麻黄碱分离度良好;线性范围依次为4.00~80.04 μg·mL^-1（r=0.999 4）,4.00~80.02 μg·mL^-1（r=0.999 3）,4.03~80.57 μg·mL^-1（r=0.999 6）,6.40~640.25 μg·mL^-1（r=0.999 6）,6.41~641.34 μg·mL^-1（r=0.999 7）;检出限依次为2.03,1.98,1.93,3.67,3.73 μg·mL^-1;定量限依次为3.98,3.87,4.03,6.37,6.41 μg·mL^-1;平均回收率依次为99.06%,98.87%,99.95%,99.92%,100.54%,RSD依次为0.95%,1.55%,1.58%,1.18%,0.91%;风湿骨痛丸中乌头碱、次乌头碱、新乌头碱、麻黄碱、伪麻黄碱的平均含量依次为0.001%,0.004%,0.004%,0.041%,0.027%。结论： 本研究UPLC方法准确,重复性良好,可测定风湿骨痛丸中乌头碱、次乌头碱、新乌头碱、麻黄碱、伪麻黄碱的含量,为风湿骨痛丸的质量控制提供参考。     

咳喘丸质量标准的建立

摘要：目的:建立咳喘丸的质量标准。方法:采用显微鉴别法鉴别处方中甘草、荆芥、炒紫苏子;采用TLC法鉴别处方中蜜麻黄、苦杏仁、甘草;采用HPLC法测定处方中盐酸麻黄碱和盐酸伪麻黄碱的含量,色谱柱:Agilent Eclipse Plus C18柱（250 mm×4.6 mm,5μm）;流动相:乙腈-0.1%磷酸溶液（3∶97）;流速:1.0 ml·min-1;检测波长:210 nm;进样量:10μl。结果:在显微鉴别中,显微特征明显,检出甘草、荆芥、炒紫苏子;在TLC鉴别中,TLC色谱斑点清晰,检出蜜麻黄、苦杏仁、甘草;盐酸麻黄碱在2.014～100.7μg·ml-1浓度范围内呈现良好的线性关系（r=1.000 0）,平均回收率为100.3%,RSD为0.80%（n=9）;盐酸伪麻黄碱在2.048～102.400μg·ml-1浓度范围内呈现良好的线性关系（r=1.000 0）,平均回收率为100.7%,RSD为1.62%（n=9）;本品每1 g含蜜麻黄以盐酸麻黄碱(C10H15NO·HCl)和盐酸伪麻黄碱(C10H15NO·HCl)的总量计,不得少于0.60 mg。结论:该方法简便、准确可靠,精密度、稳定性、重复性良好,可用于咳喘丸的质量控制。     

用HPLC法测定复方对乙酰氨基酚胶囊4组分的含量

目的 :采用HPLC法同时测定复方对乙酰氨基酚胶囊中对乙酰氨基酚、盐酸伪麻黄碱、咖啡因、和马来酸氯苯那敏的含量。方法 :色谱柱为ODSC18,15 0mm× 4 .6mm ;流动相 :甲醇 - 0 .0 5mol/L磷酸二氢钾 三乙胺 (15∶85∶0 .0 2 ) ,用磷酸调pH至 3.4 ,检测波长 2 15nm。结果 :线性范围分别为 :对乙酰氨基酚 5 0～ 35 0 μg·mL-1(r =0 .9997)、盐酸伪麻黄碱 6 .0～ 4 2μg·mL-1(r=0 .9938)、咖啡因 6 .0～ 4 2 μg·mL-1(r =0 .9998)、马来酸氯苯那敏 0 .6～ 4 .2 μg·mL-1(r =0 .9999)。平均回收率分别为 :对乙酰氨基酚 10 2 .3%、盐酸伪麻黄碱 10 0 .9%、咖啡因 10 1.8%、马来酸氯苯那敏 10 1.5 %。结论 :本法分离度好 ,快速 ,简便 ,可同时测定该胶囊中的四组分。     

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.     

Pharmacological treatment of COVID-19: an opinion paper

The precocity and efficacy of the vaccines developed so far against COVID-19 has been the most significant and saving advance against the pandemic. The development of vaccines has not prevented, during the whole period of the pandemic, the constant search for therapeutic medicines, both among existing drugs with different indications and in the development of new drugs. The Scientific Committee of the COVID-19 of the Illustrious College of Physicians of Madrid wanted to offer an early, simplified and critical approach to these new drugs, to new developments in immunotherapy and to what has been learned from the immune response modulators already known and which have proven effective against the virus, in order to help understand the current situation.     

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.