HPLC法测定复方对乙酰氨基酚片中对乙酰氨基酚、乙酰水杨酸及咖啡因的含量

目的:采用高效液相色谱法测定复方对乙酰氨基酚片中对乙酰氨基酚、乙酰水杨酸及咖啡因的含量。方法:采用 Li-chrospher C_(18)(5 μm,4.6 mm×250 mm)色谱柱,以甲醇-水-冰醋酸(40:60:0.3)为流动相,流速1.0 mL·min~(-1),检测波长272 nm,柱温35℃。结果:对乙酰氨基酚线性范围为19.93～199.32μg·mL~(-1)(r=0.9998),平均回收率(n=9)为99.2%;乙酰水杨酸线性范围为36.00～359.96μg·mL~(-1)(r=0.9999),平均同收率(n=9)为99.7%;咖啡因线性范围为4.90～49.04μg·mL~(-1)(r=0.9998),平均同收率(n=9)为98.8%。结论:方法简使,结果准确,适用于该产品的质量控制。     

HPLC法测定板蓝根药材中靛蓝和靛玉红的含量

目的:采用 HPLC—UV 法测定板蓝根中靛蓝和靛玉红含量。方法:将板蓝根经氯仿回流提取,然后用 HPLC 测定。色谱柱为 Diamonsil~(TM)C_(18)(250 mm×4.6 mm,5μm),流动相为乙腈-0.05%磷酸梯度洗脱,流速为1.0 mL·min~(-1),检测波长为300 nm,柱温为30℃。结果:靛蓝线性范围为0.1488～9.520μg·mL~(-1)(r=0.9999,n=7),平均回收率为97.8%,RSD=1.7%(n=6);靛玉红线性范围为0.2539～16.25μg·mL~(-1)(r=0.9995,n=7),平均回收率为98.5%,RSD=1.64%(n=6)。结论:所用方法准确可靠,适合于板蓝根药材的质量控制。     

HPLC测定风湿安泰片中马钱子碱和士的宁的含量

目的:采用反相高效液相色谱法测定风湿安泰片中士的宁和马钱子碱的含量。方法:采用 Hypersil BDS C_(18)色谱柱(4.6 mm×250 mm,5 μm),保护柱(4.6 mm×12 mm);乙腈-0.3%三乙胺溶液(磷酸调 pH=2.6)(10:90)为流动相,流速:1.0 mL·min~(-1),柱温:室温,检测波长:254 nm。结果:士的宁在4.6～46μg·mL~(-1)(r=0.9998),马钱子碱在2.65～26.5μg·mL~(-1)(r=0.9998)范围内呈良好的线性关系,士的宁的平均回收率(n=5)为101.1%,RSD 为2.8%;马钱子碱的平均回收率(n=5)为99.6%,RSD 为2.9%。结论:本方法准确、简便、快速,适用于风湿安泰片的质量控制。     

RP—HPLC法同时测定冠心宁冻干粉针剂中丹酚酸B和阿魏酸的含量

目的:建立了同时测定冠心宁冻干粉针剂中丹酚酸 B 和阿魏酸含量的方法。方法:采用 RP-HPLC 法,Hypersil ODS2C_(18)柱(250 mm×4.6 mm,5μm),流动相为甲醇-乙腈-1.7%甲酸水溶液(11:12:77),流速1.0 mL·min~(-1),检测波长为320nm。结果:丹酚酸 B 和阿魏酸浓度分别在1.70～25.47μg·mL~(-1)(r=0.9997,n=6)和0.05～0.68μg·mL~(-1)(r=0.9994,n=6)内与峰面积呈良好线性关系,平均回收率(n=9)分别为101.1%和99.2%。结论:测定方法准确、重复性好,为冠心宁冻干粉针剂质量评价提供可靠方法。     

HPLC法测定苦参总碱中苦参碱与氧化苦参碱的含量

目的:采用高效液相色谱法测定苦参总碱中苦参碱和氧化苦参碱的含量。方法:采用 Elite Hypersil NH_2柱(5μm,250mm×4.6 mm),乙腈-无水乙醇-3%磷酸溶液(81:10:9)为流动相,流速:1.0 mL·min~(-1),检测波长220 nm,柱温:25℃,进样量:10 μL。结果:苦参碱、氧化苦参碱的线性范围分别为5.32～53.2μg·mL~(-1)(r=0.9997),65.7～525.6μg·mL~(-1)(r=0.9995)。苦参碱平均加样回收率为99.5%,RSD=1.0%(n=6);氧化苦参碱的平均加样回收率为99.7%,RSD=0.6%(n=6)。结论:本方法操作简便、快速、可靠,可用于控制苦参总碱质量。     

氯唑西林血药浓度HPLC测定方法的研究

目的:建立氯唑西林血药浓度的高效液相色谱分析方法。方法:以苯唑西林为内标,用乙腈为沉淀剂处理人血浆样品,分析柱为 SinoChrom ODS-BP(5μm,250mm×4.6mm),流动相为0.02mol·L~(-1)磷酸二氢钠缓冲液-乙腈(65:35,用磷酸调pH 为4.6),流速1.10mL·min~(-1),柱温30℃,在225nm 波长处检测。按内标法定量。结果:血药浓度线性范围为0.25～40.0μg·mL~(-1)(r=0.9994),最低检测限0.20μg·mL~(-1)(S/N>3),提取回收率为92.5%～100.5%(n=5),方法回收率为96.2%～100.8%(n=5),日内和日间 RSD(n=5)分别为1.78%～4.05%和1.96%～7.36%。结论:本方法简便、准确、精密度高、重现性好,适用于氯唑西林人体内药代动力学研究及人体生物等效性研究。     

高效液相色谱法测定复方利血平片中4种成分的含量

目的:建立同时测定复方利血平片中硫酸双肼屈嗪、氢氯噻嗪、维生素B_1和维生素B_6含量的高效液相色谱法。方法:采用Hypersil BDS C_(18)柱(200mm×4.6mm,5μm);流动相为0.01mol·L~(-1)庚烷磺酸钠溶液-乙腈-甲醇-三乙胺(65:20:15:0.02),用5%磷酸溶液调节pH至3.6;检测波长为240nm。结果:硫酸双肼屈嗪在32.5～406.7μg·ml~(-1)(r=0.999 2),氢氯噻嗪在24.4～304.4μg·ml~(-1)(r=0.999 4),维生素B_1在8.5～106.6μg·ml~(-1)(r=0.999 3),维生素B_6在8.5～106.0μg·ml~(-1) (r=0.999 1)浓度范围内线性关系良好;硫酸双肼屈嗪回收率为100.2%,RSD为0.8%(n=9),氢氯噻嗪回收率为99.7%,RSD为1.0%(n=9),维生素B_1回收率为100.0%,RSD为0.9%(n=9),维生素B_6回收率为100.5%,RSD为0.9%(n=9)。结论:本法操作简便、快捷,结果准确,可用于复方利血平片的质量控制。     

HPLC法测定痔速宁片中芦丁与没食子酸的含量

目的建立HPLC法测定痔速宁片中芦丁与没食子酸含量的方法。方法采用Thermo Acclaim TM 120C18色谱柱(150mm×4.6mm,5μm);流动相为甲醇-0.4mL·L~(-1)磷酸溶液,梯度洗脱;流速为1.0mL·min~(-1);检测波长为257和273nm;进样量5μL;柱温35℃。结果芦丁与没食子酸的线性范围分别为10.54~105.4μg·mL~(-1)(r=0.999 9,n=6)和51.075~510.75μg·mL~(-1)(r=0.999 9,n=6);提取回收率分别为99.2%(RSD=0.7%,n=6)和99.4%(RSD=0.9%,n=6)。结论该方法简便、可靠、准确,可用于该制剂的质量控制。     

HPLC法同时测定银黄制剂中的绿原酸和黄芩苷含量

目的:建立同时测定银黄制剂中绿原酸和黄芩苷的 HPLC 方法。方法:色谱柱为 Waters Symmetry C_(18)(3.9 mm×150mm,5μm)柱,以甲醇-0.4%磷酸水溶液为流动相,梯度洗脱(0→15 min,甲醇15%→55%;15→25 min,甲醇55%;25→28min,甲醇55%→15%)。流速为0.8 mL·min~(-1),检测波长为320 nm,0.02 AUFS。结果:绿原酸的线性范围为6.88～110.08μg·mL~(-1)(r=0.9996),平均回收率为97.4%,RSD 为2.2%(n:5);黄芩苷的线性范围为13.40～214.40μg·mL~(-1)(r=0.9998),平均回收率为96.7%,RSD 为2.0%(n=5)。结论:该方法简单、快速、准确,可为银黄制剂的质量控制提供实验依据。     

HPLC法同时测定乳块消片中丹参素、原儿茶醛、橙皮苷、丹酚酸B的含量

目的:采用 HPLC 法同时测定乳块消片中丹参素、原儿茶醛、橙皮苷、丹酚酸 B 4种成分的含量。方法:采用 Eclipse XDB-C_(18)色谱柱(4.6 mm×250 mm,5μm);以甲醇-3%醋酸水溶液为流动相梯度洗脱;流速为1 mL·min~(-1);柱温为30℃;检洲波长280 nm。结果:丹参素、原儿茶醛、橙皮苷、卅酚酸 B 进样浓度分别在7.0～223.0μg·mL~(-1)(r=0.9999),0.7～21.5μg·mL~(-1)(r=0.9999),8.5～272.0μg·mL~(-1)(r=0.9999),34.8～1112.0μg·mL~(-1)(r=0.9999)范围内呈良好的线性关系;平均回收率(n=6)分别为101.4%,98.9%,96.2%,99.4%及其 RSD 分别为2.4%,1.8%,1.3%,1.5%。结论:本方法简便,重现性好,结果准确可靠,为乳块消片的质量控制奠定了基础。     

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.     

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.