HPLC法同时测定辛芩颗粒中细辛脂素、升麻素苷、5-O-甲基维斯阿米醇苷的含量

目的:建立高效液相色谱法测定辛芩颗粒中细辛脂素、升麻素苷、5-O-甲基维斯阿米醇苷含量的方法。方法:色谱柱:ZORBAX Eclipse XDB-C18柱(150 mm×4.6 mm,5μm);流速为1.0 ml·min-1;柱温:30℃;流动相:甲醇-水梯度洗脱;检测波长:0~30 min为254 nm,30~55 min为287 nm;进样量:10μl。结果:升麻素苷在浓度为10.210~163.400μg·ml-1时线性关系良好,r=0.999 7,平均回收率为100.30%,RSD为1.6%(n=6);5-O-甲基维斯阿米醇苷在浓度为10.160~162.600μg·ml-1时线性关系良好,r=0.999 8,平均回收率为101.53%,RSD为1.1%(n=6);细辛脂素在浓度为5.015~80.240μg·ml-1时线性关系良好,r=0.999 8,平均回收率为101.12%,RSD为1.2%(n=6)。结论:该方法简单、准确,同时测定3种有效成分的含量,可用于辛芩颗粒的质量控制。     

HPLC法测定鼻渊丸中木兰脂素的含量

目的:建立测定鼻渊丸中木兰脂素含量测定的HPLC方法;方法:Kromasil,C18柱(200 mm×4．6 mm,5μm),流动相为乙睛-水(38:62);检测波长:278 nm,流速:1 ml·min-1。结果:线性范围为0．27-6．78μg,平均回收率98．5％,RSD=1．4％。结论:方法简便,精密度好,可用于鼻渊丸的质量控制。     

高效液相色谱法测定鼻康喷雾剂中木兰脂素的含量

目的建立高效液相色谱法测定鼻康喷雾剂中木兰脂素的含量。方法选用Allsphere-C18色谱柱（250mm×4.6mm,5μm）,以乙腈-3.3%四氢呋喃溶液（34：66）为流动相,检测波长为278nm,柱温为30℃,流速为1.2mL.min-1。结果木兰脂素在0.0936～1.872μg范围内线性关系良好,r=0.9999。平均回收率为98.6%,RSD为1.26%。结论该方法准确可靠、精密度高、重现性好,可用于鼻康喷雾剂中木兰脂素的含量测定。     

高效液相色谱法测定中药辛夷中木兰脂素的含量

目的:建立高效液相色谱法测定中药辛夷中木兰脂素含量。方法:采用Zorbaz SB-C_8(4.6mm×150mm,5μm)柱,保护柱C_8(4.6mm×20mm,10μm),以乙腈-四氢呋喃-水(35:1:64)为流动相,流速1mL·min~(-1),检测波长为278 nm,柱温:室温。结果:木兰脂素的线性范围为0.1～1.5μg,r为0.999 9,平均回收率为97.5％,RSD为0.72％(n=5)。结论:该方法准确、简便、快速,灵敏度高,重现性好。为辛夷建立了新的质量控制方法。     

反相高效液相色谱法测定利鼻片中木兰脂素含量

目的建立测定利鼻片中木兰脂素含量的反相高效液相色谱法。方法采用UltimateTM XB-C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-四氢呋喃-水(35∶1∶64),检测波长为276 nm。结果木兰脂素进样量在0.102 8～1.028μg范围内与峰面积呈良好线性关系(r=0.999 8),平均加样回收率为97.17%,RSD为1.49%(n=6)。结论该方法简便易行、准确可靠,可用于利鼻片的质量控制。     

用微波萃取-HPLC法测定不同产地辛夷药材中木兰脂素的含量

目的:采用微波萃取-HPLC法测定木兰脂素的含量,并考察4个不同产地辛夷药材中木兰脂素的含量差异。方法:采用微波萃取法,以75%乙醇为溶剂,在76℃恒温800 s萃取辛夷药材中的木兰脂素。Shim-Pack VP-ODS柱(150 mm×4.6 mm,5μm),流动相:乙腈-水(40∶60),流速:0.8 ml/min;柱温:室温,检测波长:238 nm,采用HPLC法测定木兰脂素的含量。结果:以峰面积(A)对浓度(c)作线性回归,回归方程为A=2.922 7×104c-3 617.4(r=0.999 9),在5.6~240.8μg/ml浓度范围内,木兰脂素的峰面积与浓度呈良好线性关系。该法的精密度、重现性和稳定性良好,低、中、高浓度(104.87、127.42和172.51μg/ml)的加样回收率分别为(100.39±1.58)%(、103.82±4.04)%和(103.74±0.13)%(n=3)。采用该法测得河南、河北、湖南、湖北4地所产的辛夷药材中木兰脂素含量分别为(6.59±0.39)%(、3.44±0.48)%、(2.73±0.28)%和(4.18±0.25)%(n=3)。其中河南产辛夷药材中木兰脂素含量最高。结论:本方法简便、准确、稳定、重复性好,可作为辛夷药材及相关制剂质量控制的定量方法。     

木兰脂素在大鼠体内的药动学研究

目的:研究木兰脂素在大鼠体内的药动学特征。方法:采用高效液相色谱(HPLC)法。色谱柱为Kromasil C18,流动相为乙腈-四氢呋喃-水(39∶1∶60),流速为1.0 ml/min,检测波长为278 nm,柱温为35℃,进样量为20μl。8只Wistar大鼠于给药[10mg(生药)/kg]前及给药后0.25、0.5、0.75、1、1.5、2、4、8、12、20 h尾静脉断尾取血测定血药浓度,采用DAS2.1.1软件计算药动学参数。结果:木兰脂素检测质量浓度线性范围为0.05~10.00μg/ml(r=0.999 5),精密度、稳定性试验的RSD均小于13%(n=6),方法回收率为97.32%~102.15%(n=6),提取回收率为84.63%~90.02%(n=6)。木兰脂素在大鼠体内t1/2α为(0.48±0.22)h,t1/2β为(7.96±2.57)h,CL/F为(0.09±0.032)L/(h·kg),AUC0-20 h为(944.43±212.83)mg·h/L。结论:本方法精密度、稳定性、准确度均符合生物样品测定要求。木兰脂素在大鼠体内AUC0-20 h与剂量呈良好的线性关系,过程符合二室模型。     

HPLC法同时测定肿痛安胶囊中5种成分的含量

目的建立同时测定肿痛安胶囊中:天麻素、升麻素苷、5-O-甲基维斯阿米醇苷、欧前胡素和异欧前胡素含量的HPLC法。方法色谱柱:Phenomenex Luna C_(18)柱(250mm×4.6mm,5μm);流速:1.0mL·min~(-1);柱温:25℃;流动相:甲醇-水梯度洗脱;检测波长:230nm;进样量:5μL。结果天麻素质量浓度在12.46～199.30μg·mL~(-1)范围内线性关系良好,r_1=0.999 5,平均回收率为101.2%,RSD值为1.6%(n=6);升麻素苷质量浓度在12.07～193.20μg·mL~(-1)范围内线性关系良好,r_2=0.999 7,平均回收率为100.1%,RSD值为1.8%(n=6);5-O-甲基维斯阿米醇苷质量浓度在8.12～129.90μg·mL~(-1)范围内线性关系良好,r_3=0.999 8,平均回收率为99.1%,RSD值为1.7%(n=6);欧前胡素质量浓度在12.52～200.40μg·mL~(-1)范围内线性关系良好,r_4=0.999 6,平均回收率为98.6%,RSD值为1.4%(n=6);异欧前胡素质量浓度在12.65～202.40μg·mL~(-1)范围内线性关系良好,r_5=0.999 6,平均回收率为99.0%,RSD值为0.7%(n=6)。结论该方法简单、准确,可同时测定5种成分的含量,可用于肿痛安胶囊的质量控制。     

HPLC法测定生血颗粒中补骨脂素、异补骨脂素的含量

目的:建立HPLC法测定生血颗粒中补骨脂素和异补骨素的含量。方法:色谱柱为SB-C_(18)柱(250mm×4.6mm,10μm);柱温:40℃;流动相为甲醇-水(50:50);流速为1.0ml·min~(-1);检测波长为246nm。结果:补骨脂素在1.135～45.400μg·ml~(-1)范围内、异补骨脂素在1.035～41.400μg·ml~(-1)范围内呈良好的线性关系(相关系数分别为r=0.999 9和r=1.000 0),平均回收率分别为97.05%和96.36%(RSD分别为0.78%和0.86%,n=6)。结论:所建立的方法稳定性可靠、灵敏,结果准确,可用于生血颗粒的质量控制。     

HPLC法测定通窍鼻炎片中木兰脂素的含量

目的建立HPLC法测定通窍鼻炎片中木兰脂含量的分析方法。方法用Phenomenex C18色谱柱(250mm×4.6mm,5μm),乙腈-四氢呋喃-水(35∶1∶64)作为流动相,流速为1.0ml.min-1,检测波长为274nm。结果木兰脂素在0.2~2.0μg与峰面积线性关系良好(r=0.9999),平均回收率为99.77%,RSD=1.048%(n=5)。结论方法操作简便、重现性好、灵敏度高、专属性强,可用于通窍鼻炎片的质量控制。     

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.