HPLC梯度洗脱法测定丙泊酚中/长链脂肪乳注射液的含量及有关物质

目的：建立测定丙泊酚中/长链脂肪乳注射液中的丙泊酚及其有关物质的HPLC方法。方法：色谱柱为Waters XBridge RP18柱（4.6mm×150mm,5μm）;流动相为磷酸二氢钠溶液-乙腈,梯度洗脱;柱温为40℃;检测波长为275nm和254nm。丙泊酚的测定采用外标法,有关物质检查采用外标法与自身对照法。结果：丙泊酚与其两杂质能较好分离,相邻各峰间分离度均大于1.5;丙泊酚、杂质Ⅰ和杂质Ⅱ的线性范围分别为97.2~1457.9μg?mL-1（r=0.999 9）、0.11～1.57μg?mL-1（r=0.999 9）和0.11～1.59μg?mL-1（r=0.999 9）;平均回收率（n=9）分别为99.2%（RSD＝1.4%）、105.8%（RSD＝1.5%）和96.7%（RSD＝4.8%）。结论：所建方法简便快速、专属性强、重复性好,可用于丙泊酚中/长链脂肪乳注射液的含量测定和杂质检查。     

肝纤维化食蟹猴血浆丙泊酚浓度的HPLC测定

目的 建立血浆丙泊酚浓度的高效液相色谱(HPLC)测定方法,探讨肝纤维化食蟹猴丙泊酚血浆浓度变化.方法 选择肝纤维化S0、S1、S2、S3、S4期的雄性食蟹猴各12只,持续输注丙泊酚8mg·kg-1·h1 30min.于输注1、10、20、30 min和苏醒时采血,采用Agilent 1100型HPLC仪测定血浆丙泊酚浓度.血浆样品经6％高氯酸沉淀蛋白处理;色谱柱为Hypersil C18,流动相为甲醇-水(68∶32);流速1 ml/min;紫外检测波长为258 nm;柱温为室温;内标为麝香草酚,进样量:20μl.结果 丙泊酚与血浆中其他成分分离良好,在0.1-10 μg/ml范围内线性关系良好,回归方程为Ai/As=0.23C-0.045(r=0.995,n=5).方法回收率为98.69％ 100.10％,提取回收率为86.86％-89.48％.日内、日间精密度均小于5％.S4期肝纤维化组各时间点的血浆丙泊酚浓度均高于S0-S3期(P＜0.05).结论 HPLC法检测血浆丙泊酚浓度,灵敏度高,结果准确.丙泊酚代谢随食蟹猴肝纤维化程度加重而减慢.     

高效液相色谱法测定人血清中丙泊酚含量

目的：建立人血清中丙泊酚的HPLC测定方法,为其药代动力学研究和临床疗效研究奠定方法学基础。方法：色谱柱：TIANHE Kromasil C18柱（200mm×4．6mm,5μm）;流动相-乙腈-甲醇-水（10：60：30）;pH7（正丁胺0．1％,冰醋酸0．15％）;柱温：室温;流速：0．7ml／min;紫外检测波长：273nm;进样量：50μl;内标法测定丙泊酚的血药浓度。结果：丙泊酚与血清中其他组分分离良好,血清中丙泊酚在0．05—100μg／ml范围内呈现良好线性关系,得出回归方程Y=0．0002X-0．0786（r=0．9996）,方法回收率为96,72％,日内和日间RSD均小于10％。结论：本实验建立的HPLC方法简单、准确,适用于血清中丙泊酚浓度测定。     

UPLC法测定丙泊酚注射液中丙泊酚的含量及有关物质

目的：建立超高效液相色谱法（UPLC）测定丙泊酚注射液中丙泊酚含量及有关物质。方法：采用UPLC法对丙泊酚注射液中的丙泊酚及其有关物质进行定量分析,色谱柱为Acquity UPLC@BEH C18（50 mm×2.1 mm,粒直径1.7μm）;流动相为磷酸二氢钠溶液-乙腈,梯度洗脱;流速为0.2 mL·min-1;柱温为30℃;检测波长为275 nm。结果：丙泊酚在51.18~2559 mg· L-1、2,6-二异丙基-1,4-苯醌在0.501~100.2 mg·L-1、3,3’,5,5’-四异丙基联苯酚在0.498~99.6 mg·L-1范围内,均线性关系良好（r≥0.99）,稳定性试验的RSD 为0.52%（n=6）,方法重复性的RSD为0.33%（n=6）,丙泊酚的加样回收率为99.0%,RSD为0.83%（n=6）。结论：该UPLC法快速、灵敏,结果准确,适用于丙泊酚注射液的质量控制。     

高效液相色谱法同时测定复方咽炎喷雾剂中3种药物含量

目的:建立HPLC法同时测定喷雾剂中的地塞米松磷酸钠、醋酸氯己定、甘草酸二铵含量的方法。方法:色谱柱为Diamonsil C18柱(250 mm×4.6 mm,5μm),流动相为0.01 mol.L-1磷酸溶液(用三乙胺调pH 2.8)-乙腈(68∶32)。柱温30℃,检测波长为250 nm。结果:地塞米松磷酸钠、醋酸氯己定、甘草酸二铵的分离度均>1.5,理论塔板数均>2 000;回归方程依次分别为:y=43 811x+180 553(r=0.999 5);y=23 956x+107 969(r=0.999 6);y=16 423x-56 524(r=0.999 5);线性范围分别为10～200μg.mL-1,10～200μg.mL-1,25～500μg.mL-1。结论:本法操作方便,结果准确可靠,可用于复方咽炎喷雾剂中的地塞米松磷酸钠、醋酸氯己定、甘草酸二铵含量测定。     

丙泊酚或七氟烷麻醉单肺通气中初始呼吸末CO2差异与最低动脉血氧分压值关联的研究

目的：研究丙泊酚或七氟烷麻醉单肺通气早期阶段呼吸末CO2差异（ETCO2）与最低PaO2值的关联。方法：36例择期胸科手术患者被随机分成P组（给予丙泊酚维持麻醉,n=18）和S组（给予七氟烷维持麻醉,n=18）两组。在FiO2=0.9时,测量双肺通气和单肺通气后5min、15min、30min和45min的动脉血气以及单肺通气前和后5min ETCO2值。结果：单肺通气中每组最低PaO2值（x）与初始ETCO2差异（y）有显著负相关性（P组;y=-0.0203x＋7.2571,r2=0.5351;S组;y=-0.0257x＋7.3158,r2=0.6129）。组间比较没有显著差异。结论：本研究表明双肺通气和单肺通气早期阶段ETCO2差异与单肺通气中损害的氧合功能相关。因此在丙泊酚或七氟烷麻醉单肺通气中最低PaO2值是一个简单、方便的预测氧合功能指标。     

UPLC测定不同产地半夏药材及其炮制品中的草酸钙

目的 采用UPLC法测定半夏药材及其炮制品中草酸钙的含量.方法 色谱柱为Acquity UPLC BEH C18柱(50 mm×2.1 mm,1.7 μm),流动相为0.5％ (NH4)H2PO4缓冲液(磷酸调pH2.8),流速0.5 mL· min-1,柱温30 ℃,检测波长210 nm.结果 线性方程为:y=1.8488×104X+4.146×103(r=0.9999),2.58 ～ 25.80 μg· mL-1草酸与峰面积的线性关系良好,平均加样回收率为98.58％,RSD=1.01％(n=9).结论 所用方法准确可靠,可为半夏药材的质量控制提供参考.     

用RP-HPLC法测定靶控输注下血浆中的丙泊酚浓度

目的：建立测定靶控输注下血浆中丙泊酚浓度的方法。方法：采用RP-HPLC法,色谱柱：Shim-pack CLCODS-C18柱;流动相：乙腈∶水=65∶35,流速：1.5ml/min;检测波长：220nm;柱温：25℃。结果：丙泊酚在0.05～5.0μg/ml范围内线性关系良好（r=0.999 8）,精密度和稳定性良好,低、中、高浓度（0.5、2.0、5.0μg/ml）丙泊酚的回收率分别为（103.0±2.5）%、（98.0±1.4）%和（102.5±3.1）%（n=3）。结论：该方法准确、灵敏、快捷,可用于测定靶控输注下血浆中的丙泊酚浓度。     

反相高效液相色谱法测定丙泊酚血药浓度

目的 :建立测定丙泊酚人血药浓度的反相高效液相色谱 荧光检测分析方法。方法 :使用Agi lent 110 0型高效液相色谱仪、PhenomenexSecurityGuard ( 4mm× 3mm )保护柱、DiamonsilC18( 15 0mm× 4 .6mm ,5 μm)色谱柱。在血样中加入麝香草酚 (内标 )的甲醇溶液沉淀蛋白后 ,离心取上清液 ,进行HPLC分析。流动相 :乙腈∶水 =5 6∶4 4(V/V) ;流速 :1.5mL·min- 1;荧光检测 :λex=2 76nm ,λem=312nm。结果 :本法标准曲线线性方程为Y =1.787C - 0 .0 31(r =0 .9997,n =9,线性浓度范围为 0 .0 2～ 8.0mg·L- 1) ;最低检测浓度为 4 μg·L- 1(S/N =2 ) ;平均方法回收率为 98.71%;日内、日间精密度RSD( %)均小于 4 .2 %。结论 :本方法简便、灵敏、准确 ,可用于临床上丙泊酚的血药浓度监测。     

HPLC法测定复方罗布麻片中防己诺林碱与粉防己碱的含量

目的 用高效液相色谱(HPLC)法测定复方罗布麻片中防己诺林碱与粉防己碱的含量,控制药品中防己的含量.方法 色谱柱为Hypersil ODS 2 (5 μm, 4.6 mm×250 mm);流动相为乙腈-甲醇-水-冰醋酸(49:23:28:1)(每100 ml含十二烷基硫酸钠0.41 g);流速为1.0 ml/min;检测波长为280 nm;柱温为35℃.进样量为10 μl.以甲醇为溶剂超声30 min处理提取复方罗布麻片中防己诺林碱与粉防己碱.结果 防己诺林碱在19.04～304.64 μg/ml范围内线性关系良好,回归方程为y=7 758.4x-3.471 9(r=1.000 0,n=5),回收率为99.3%(n=6).粉防己碱在16.16～258.56 μg/ml范围内线性关系良好,回归方程为y=6 194.4x-0.238 4(r=1.000 0,n=5),回收率为99.4%(n=6).结论 该法能准确测定复方罗布麻片中防己诺林碱与粉防己碱的含量.     

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.