高效液相色谱法同时测定古方生化汤中阿魏酸和川芎嗪的含量

目的:建立用反相高效液相色谱法同时测定古方生化汤中阿魏酸和川芎嗪含量的方法.方法:以甲醇-水(含1%的冰醋酸),(7:18)为流动相,Zorbax C18柱(250 mm×4.6 mm,5 μm)为固定相,紫外检测波长为280 nm,外标法定量.结果:阿魏酸和川芎嗪分离完全,阿魏酸在8.06～64.48 mg·L-1的浓度范围内回归,方程为Y=1811.32 1170.33X,r=0.9954,平均回收率为97.9%,RSD为1.4%;川芎嗪在4.03～20.15 mg·L-1的浓度范围内,回归方程为Y=16.60 1401.94X,r=0.9941,平均回收率为101.9%,RSD为2.6%.结论:此法快捷、简便,准确,可作为生化汤的质量标准.     

HPLC测定九味羌活丸中阿魏酸的含量

目的:建立高效液相色谱法测定九味羌活丸中阿魏酸含量方法。方法:色谱柱为Kromasil C18柱,流动相为甲醇-水-冰醋酸(25∶75∶0.65),检测波长为320nm,流速1.0ml/min。结果:阿魏酸的回归方程为Y=28.486X-1.1455,r=0.9996(n=6),平均回收率98.72%,RSD为0.73%(n=6)。结论:该法结果准确,专属性强,可将其作为九味羌活丸质控指标之一。     

RP-HPLC测定阿戈美拉汀原料药的含量

目的 采用RP-HPLC法测定阿戈美拉汀原料药的含量.方法 色谱柱为Plastil-C_(18)柱(150 mm×4.6 mm,5 μm),流动相为乙腈-水(30:70),流速1.0 mL·min~(-1),检测波长为230 nm.结果 线性回归方程为:Y=2.283×10~4X-1.353×10~4(r=0.9999),线性范围为5～80 μg·mL~(-1),平均回收率为100.4%(n=9),RSD=0.97%.结论 所建方法简便、快速、灵敏度高,可用于阿戈美拉汀原料药的含量测定.     

高效液相色谱法测定注射用复方粉针剂中地塞米松磷酸钠和去甲万古霉素的含量

目的建立高效液相色谱法同时测定复方粉针剂中地塞米松磷酸钠和去甲万古霉素的含量.方法采用SphereSorb C18色谱柱(4.6mm×250mm,10μm),甲醇-0.01mol·L-1磷酸氢二铵(20:80,磷酸调pH6.0)为流动相,检测波长:214nm,流 /min,柱温为30℃,进样量20μL.结果地塞米松磷酸钠线性范围为9.6～48mg·L-1,回归方程Y=30605.3X速:1.0mL16315.8,r=0.9999,平均回收率98.1%,RSD为0.92%(n=9);去甲万古霉素线性范围20～100mg·L-1,回归方程Y=5171.6X-8435.4,r=0.9993,平均回收率100.5%,RSD为1.0%(n=9).结论方法简便、可靠、结果准确,可用于本制剂的含量测定和质量控制.     

HPLC法测定参芪生肌颗粒中阿魏酸的含量

目的:采用HPLC法测定参芪生肌颗粒中阿魏酸的含量.方法:采用70%甲醇超声提取,HPLC法测定.Kromasil C18柱(150 mm×4.6 mm,5 μm)分离;柱温30℃;流动相为甲醇-0.1%磷酸溶液(30:70);流速为1.0 ml·min-1;检测波长为320 nm.结果:阿魏酸的线性范围为1.578～9.468 μg(r=0.999 8);平均回收率为99.34%,RSD为1.2%(n =9).结论:方法简便、快速准确、灵敏度高,重复性好.     

HPLC法同时测定阿咖片中咖啡因、阿司匹林、游离水杨酸的含量

目的:HPLC法测定阿咖片中咖啡因、阿司匹林及游离水杨酸的含量.方法:采用Phenomenex十八烷基硅烷键合硅胶柱;流动相:1%冰醋酸(用三乙胺调节pH至3.5)-甲醇(70:30);检测波长:280 nm;流量:1.0 mL*min-1.结果:咖啡因的线性范围9.0～108.0μg·mL-1,回归方程为Y=4.97×107X-8.5×103,r=0.9999,平均回收率为100.0%,RSD为0.3%;阿司匹林的线性范围7.5～900.0 μg·mL-1,回归方程为Y=4.60×106X+9.3×104,r=0.9999,平均回收率为99.8%,RSD为1.1%;水杨酸的线性范围3.0～3.6μg·mL-1,回归方程为Y=3.00×107X-3.4×104,r=0.999 8,平均回收率为101.6%,RSD为0.98%.结论: 该方法简便,结果准确.     

高效液相色谱法测定利福肼片的含量

目的建立高效液相色谱(HPLC)法测定利福肼片含量的方法.方法HPLC法,以岛津C18(4.6 mm×150mm,5μm)色谱柱,流动相为0.02 mol·L-1磷酸氢二钠溶液(磷酸调节pH 4.5)-甲醇(25∶75,v/v),检测波长为254 nm.结果线性范围及回归方程利福平10～250 mg·L-1,Y=6.121X-1.756 2(r=0.999 0);异烟肼5～125 mg·L-1,Y=4.261 24X-2.382 6(r=0.999 7);平均回收率利福平99.08%,RSD为1.02%(n=6);异烟肼99.75%,RSD为1.17%(n=6).结论本法专属性强,准确,灵敏,可作为利福肼片含量测定的方法.     

高效液相色谱法测定接骨七厘片中阿魏酸的含量

目的 建立接骨七厘片中阿魏酸的含量测定方法.方法 采用HPLC法,shimpack vp-ODS色谱柱(4.6mm×250 mm,5 μm);流动相:甲醇-水-磷酸(48∶52∶0.2);检测波长:274 nm;流速:1.0 mL·min-1.结果 峰面积对进样量的回归方程为Y=1.635×106X 2.517×102,r=0.999 9(n=5),阿魏酸的进样量在0.096～0.48 μg线性关系良好,平均加样回收率为98.59%(n=5),RSD=1.05%.结论 该方法简便可行,准确可靠.     

高效液相色谱法测定白癜精药散中补骨脂素和异补骨脂素的含量

目的:建立白癜精药散的补骨脂素和异补骨脂素的含量测定方法.方法:高效液相色谱法,色谱柱为Agilent Zoxbox C18柱(5μm,4.5 mm×250mm);流动相为甲醇-水(47:53);检测波长为245 nm;柱温为35℃;流速为1.0 mL/min.结果:补骨脂素线性范围是0.216～1.08μg,回归方程为Y=1.264×10-7X-7.713×10-4,r=0.999 9(n=5);异补骨脂素线性范围是0.228～1.14μg,回归方程为Y=1.313×10-7X-3.008×10-4,r=0.999 8(n=5).补骨脂素与异补骨脂素的平均回收率分别为99.2%与99.1%,RSD分别为1.93%和1.87%(n=5).结论:高效液相色谱法简便、快速、灵敏、准确,重现性好.     

HPLC法同时测定排石利胆颗粒中绿原酸和龙胆苦苷的含量

目的建立高效液相色谱法同时测定排石利胆颗粒中绿原酸和龙胆苦苷的含量。方法色谱柱:DiamonsilC18柱(4.6 mm×250 mm,5μm);流动相:甲醇-1%醋酸溶液(21∶79);流速:0.9 mL.min-1;柱温:25℃;检测波长:280nm。结果在32.512～325.12μg的范围内,绿原酸的进样量与峰面积呈良好的线性关系,其回归方程为Y=1 546.2X-1 904,r=0.999 9,平均回收率为100.314%,RSD=0.5%(n=6);在98.496～984.86μg的范围内,龙胆苦苷的进样量与峰面积呈良好的线性关系,其回归方程为Y=1 413.7X-9 226.2,r=1.000,平均回收率为99.527%,RSD=0.6%(n=6)。结论本方法操作简单,准确、专属性强、重现性好,可作为制订排石利胆颗粒质量标准的依据。     

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.