不同厂家色谱柱对注射用氢化可的松琥珀酸钠与相关物质分离效果的考察

目的:比较不同厂家色谱柱对注射用氢化可的松琥珀酸钠与相关物质的分离效果,并筛选出适用于注射用氢化可的松琥珀酸钠分析的色谱柱。方法:以不同配比的磷酸盐缓冲液(pH 5.0)和甲醇为流动相,流速1.0 mL.min-1,检测波长为242nm。结果与结论:通过调整流动相的配比,Kromasil填料的色谱柱均可使17-氢化可的松琥珀酸钠、21-氢化可的松琥珀酸钠、游离氢化可的松及其他有关物质得到良好分离,且各峰的相对保留时间均符合中国药典的要求。     

HPLC法测定注射用氢化可的松琥珀酸钠（无菌粉）有关物质

目的：建立注射用氢化可的松琥珀酸钠（无菌粉）有关物质的反相高效液相色谱（HPLC）测定方法。方法：采用AlhimaC18（4．6mm×250mm,5μm）色谱柱;流动相为乙腈-水-磷酸（320：680：1）;流速1．0ml／min;检测波长254nm;柱温40℃。结果：该色谱条件下,主成分与有关物质及各降解产物能达到有效分离,单个杂质及其他总杂质量均低于限量要求。结论：该方法可用于注射用氢化可的松琥珀酸钠（无菌粉）有关物质的测定。     

RP-HPLC法同时测定人血清中内源氢化可的松与可的松的含量

目的:建立测定人血清中内源性氢化可的松与可的松含量的方法。方法:采用迪马Diamonsil C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相:乙腈-水-甲醇(51:136:77);流速:1.2 ml·min~(-1);紫外检测波长:245 nm;柱温:30℃;进样量:30μl。结果:氢化可的松在50.0～300.0μg·L~(-1),可的松在10.0～100.0μg·L~(-1)的浓度范围内线性关系良好。氢化可的松与可的松的方法回收率分别为(101.83±1.19)%和(100.52±5.91)%。92名健康者血清中氢化可的松、可的松的浓度分别为(111.60±27.30)和(18.66±4.44)μg·L~(-1),其比值为(6.08±1.10)。结论:本法操作简便,灵敏度高,快速可靠,适用于氢化可的松与可的松含量的测定,为研究人体肝脏11β-羟基类固脱氢酶(11β-HSD)的活性及调整激素治疗方案提供有效的分析手段。     

高效液相色谱法用于氨酚曲马多片质量控制的研究

目的:建立氨酚曲马多片有关物质及含量测定的 HPLC 分析法。方法:采用 Supelcosil LC-8-DB 柱(150 mm×4.6mm,5 μm),柱温40℃,以流动相 A-B[A:以磷酸调节 pH 为2.7±0.1的0.02 mol·L~(-1)磷酸二氢钾溶液-甲醇(4:1);B:以磷酸调节 pH 为2.7±0.1的0.02 mol·L~(-1)磷酸二氢钾溶液-甲醇(1:4)]线性梯度洗脱,流速:2.0 mL·min~(-1),检测波长:215 nm,用于盐酸曲马多含量及其有关物质的测定;采用 Supelcosil LC-8-DB柱(150 mm×4.6 mm,5 μm),柱温40℃,以流动相 C-D[C:0.02 mol·L~(-1)磷酸二氢钾溶液-0.02 mol·L~(-1)磷酸氢二钾溶液-甲醇(9:9:4);D:0.02 mol·L~(-1)磷酸二氢钾溶液-0.02 mol·L~(-1)磷酸氢二钾溶液-甲醇(5:5:90)]线性梯度洗脱,流速:1.0 mL·min~(-1),检测波长:215 nm,用于对乙酰氨基酚含量及其有关物质的测定。结果:在选定的色谱条件下,2种主药及其有关物质均能得到较好的分离,在测定范围内具有良好的线性、精密度及回收率。结论:此方法准确、简便、快速,两色谱系统结合,分别用于2种主药及其有关物质的定量测定,可在较高水平上控制本品质量。     

高效液相色谱法同时测定丁苯乳膏中两组分的含量

应用高效液相色谱法同时测定丁苯乳膏中丁酸氢化可的松和盐酸苯海拉明含量.色谱条件为:色谱柱:XTerra RP C18(250 mm×4.6 mm,5 mm);流动相:甲醇-乙腈-0.5％醋酸铵溶液(35∶27∶38);流速:1.0 mL·min-1;检测波长:232 nm.丁酸氢化可的松及盐酸苯海拉明在125～250 μg· mL-1及25～50 μg·mL-1范围内线性关系良好,表明应用HPLC法可同时测定该制剂丁酸氢化可的松及盐酸苯海拉明的含量.     

RP-HPLC测定氧氟沙星氢化可的松滴耳液的含量

目的:建立氧氟沙星氢化可的松滴耳液含量测定的方法。方法:采用RP-HPLC法测定滴耳液中氧氟沙星与氢化可的松的含量。色谱柱为Poresphere C_(18)(150 mm×4.6 mm,5μm);流动相为甲醇-0.025 mol·L~(-1)磷酸溶液(用三乙胺调pH至3.0)(55:45);流速0.8 ml·min~(-1);检测波长为240 nm;检测灵敏度为0.16AUFS,进样量20μl。结果:氧氟沙星在30～480μg·ml~(-1)浓度范围内,峰面积与浓度的线性关系良好(r=0.999 9),平均回收率为99.8%;氢化可的松在5～80μg·ml~(-1)浓度范围内,峰面积与浓度的线性关系良好(r=0.999 9),平均回收率为99.9%。结论:本方法快速、简便,精密度好,重复性好,可作为氧氟沙星氢化可的松滴耳液的含量测定方法。     

高效液相色谱中流动相pH值对氢化可的松琥珀酸钠保留行为的影响

目的:考察高效液相色谱中流动相pH值的变化对氢化可的松琥珀酸钠保留行为的影响。方法:色谱柱为VarianC18,流速为1.0mL.min-1,柱温为40℃,检测波长为242nm,进样量为20μL,流动相为甲醇-磷酸盐缓冲液(8mmol.L-1磷酸二氢钾液,43∶57,临用前用8mmol.L-1磷酸氢二钾溶液调节pH值分别为5.0、5.2、5.6、6.0)。结果:流动相pH值的变化仅改变氢化可的松琥珀酸钠和游离氢化可的松的保留时间,不改变其出峰顺序,当pH值为5.2时氢化可的松琥珀酸钠峰形及与游离氢化可的松分离较好,对称度在0.95~1.05之间。结论:本方法可为常用药物色谱行为规律的基础性系统研究提供依据。     

反相高效液相色谱法测定阿德福韦酯的含量及其有关物质

目的:建立反相高效液相色谱法测定阿德福韦酯含量及其有关物质。方法:采用 Inertsil C_8硅烷键合硅胶为填料的色谱柱(250 mm×4.6 mm,5 μm);以乙腈-25 mmol·L~(-1)磷酸二氢钾溶液(pH 6.0)(40:60)为流动相,流速1.0 mL·min~(-1),检测波长为262 nm。结果:杂质及降解产物能与阿德福韦酯基线分离;浓度存10.28～154.20μg·mL~(-1)范围内与峰面积呈良好线性关系,r=1.0000(n=8);最低柃测限为0.04 ng。结论:本法准确、简便,适用于阿德福韦酯及其有关物质的含量测定。     

反相高效液相色谱法测定注射用氢化可的松琥珀酸钠的含量

目的:采用反相高效液相色谱法测定注射用氢化可的松琥珀酸钠中21-氢化可的松半琥珀酸钠、17-氢化可的松半琥珀酸钠与游离氢化可的松的量.方法:ODS柱(4.0×250mm,10μm),流动相为甲醇:磷酸盐缓冲液,用0.008mol/L K2HP04溶液调节0.008mol/L KH2 P04溶液至pH=5.0)(43 : 57),检测波长242nm,流速1.0ml/min,柱温40℃.结果:氢化可的松琥珀酸钠的平均回收率99.68%.RSD为0.26%,氢化可的松琥珀酸钠在0.16～1.44μg浓度范围内呈良好线性,r=0.9999.游离氢化可的松在0.240～0.560μg浓度范围内呈良好线性,r=0.9999.结论:该方法快速、准确、灵敏,并能更好地控制药品质量.该方法已被中国药典2000年版2002增补本收载.     

RP—HPLC法测定注射用奈达铂含量及有关物质

目的:建立测定注射用奈达铂含量及其有关物质的反相高效液相色谱法。方法:采用 Shim—pack CLC—ODS 不锈钢柱(150 mm×4.6mm,5μm)为色谱柱,以甲醇-0.01 mol·L~(-1)枸橼酸溶液(用三乙胺调节 pH 至6.0)(30:70)为流动相,流速:0.7 mL·min~(-1),检测波长:220 nm,柱温:30℃。结果:奈达铂进样量在0.8～7.8μg范围内呈良好线性关系,r=0.9999。平均回收率(n=9)为99.81%。结论:该方法简便、准确、专属,可用于注射用奈达铂的含量及有关物质的测定。     

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.     

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.