卡铂及其制剂的含量测定和稳定性试验

采用反相高效液相色谱法对卡铂及其制剂的含量进行测定。色谱柱：ＹＷＧ－Ｃ１８（４．６ｍｍ×２５０ｍｍ，１０μｍ）；流动相：水（流速１ｍｌ·ｍｉｎ－１）；检测波长：２１０ｎｍ，用尿苷作内标物。在上述色谱条件下，供试品和内标物能在较短时间内完全出峰（卡铂和尿苷的保留时间分别为６．５ｍｉｎ和１０．５ｍｉｎ），且达到较好的分离（Ｒ＝３．５）。该法专一、灵敏、精密，日内和日间相对标准偏差分别为３．２％和４．３％（ｎ＝５），适用于常规分析。稳定性试验结果表明，注射用卡铂在室温（４０℃）和冷藏（４℃～１０℃）避光条件下存放两年，其含量基本保持不变。     

HPLC法测定小建中颗粒中芍药苷和肉桂酸的含量

目的：采用高效液相色谱法测定小建中颗粒中芍药苷和肉桂酸的含量。方法采用Ultimate XB－C18（4．6×250mm,5μm）色谱柱;乙腈－水（17∶83）为流动相;流速1．0mL? min －1;检测波长230nm,柱温：30℃。结果芍药苷和肉桂酸在20－200μg? mL －1（r＝0．9999）,0．2～20μg?mL －1（ r＝0．9997）范围内线性关系良好,平均加样回收率为101．58％、99．52％, RSD 分别为2．43％（ n ＝6）和2．23％（ n ＝6）。结论本法简便、准确,可作为该制剂的质量控制方法。     

HPLC法测定越鞠保和丸中阿魏酸和栀子苷的含量

目的：建立采用高效液相色谱法同时测定越鞠保和丸中栀子苷和阿魏酸的含量的方法。方法色谱柱用十八烷基硅烷键合硅胶为填充剂（Thermo Fisher Hypersil ODS,4．6mm ＆#215;250mm,5μm）。 HPLC反相法进行分离,紫外检测器检测,流动相为乙腈－0．2％醋酸溶液（20∶80）。流速：0．8mL· min －1,检测波长：0min～10min为239nm,10．01min～36min为324nm。进样：10μL。结果栀子苷和阿魏酸的保留时间分别约为6．6min、13．1min,与各自相邻峰的分离度均＞1．5。以峰面积（y）对进样浓度（x）线性回归,栀子苷回归方程：y＝15898x－33319,r＝0．9998,线性范围11．36～454．4μg· mL －1。阿魏酸回归方程：y＝81014x－51055,r＝0．9999,线性范围：3．05～243．6μg· mL －1。栀子苷和阿魏酸回收率（ n＝6）分别为99．8％和100．3％、RSD分别为0．26％和0．5％。结论本方法操作简便、准确、重现性好,可用于同时测定越鞠保和丸中栀子苷和阿魏酸的含量。     

HPLC-ELSD 法测定金线草中β-谷甾醇和胡萝卜苷含量

目的：建立同时测定金线草中β-谷甾醇和胡萝卜苷的 HPLC 方法。方法采用 HPLC-ELSD 法,色谱柱以十八烷基硅烷键合硅胶为填充剂（250 mm ×4．6 mm,5μm）,甲醇—水（96∶4）为流动相洗脱,体积流量1．0 mL·min －1,柱温30℃,漂移管温度70℃,载气体积流量1．8 L·min －1,进样体积10μL。结果β-谷甾醇和胡萝卜苷分别在0．1528～1．910μg（r ＝0．9995）和0．1016～1．270μg（r ＝0．9993）有良好的线性关系;平均回收率为99．7％和98．9％,RSD 分别为1．4％和1．8％（n ＝5）。结论该方法能准确测定金线草中β-谷甾醇和胡萝卜苷的含量。     

HPLC法快速测定艾附暖宫丸中芍药苷的含量

目的：建立快速测定艾附暖宫丸中芍药苷含量的液相色谱法。方法采用 Bonshell ASB C18表面多孔壳层色谱柱（4．6×150mm,2．7μm）,按照中国药典2010年版一部中艾附暖宫丸含量测定方法,以乙腈－0．1％磷酸溶液（12∶88）为流动相,等度洗脱,流速1．0mL· min －1,柱温30℃,检测波长230nm。结果样品溶液色谱图中显示与对照品溶液色谱图中相同的芍药苷色谱峰,且分离度良好。芍药苷在0．5～100．0μg· mL －1范围内与峰面积呈良好的线性关系（r＝0．9985）;重复性试验的 RSD＝1．4％（n＝6）;平均回收率为96．4％,RSD＝0．85％（n ＝6）。结论该方法快速、简便、灵敏、专属性强,可以实现艾附暖宫丸中芍药苷含量的快速检测。     

HPLC法同时测定颈舒颗粒中天麻素和桂皮醛的含量

目的：建立HPLC法同时测定颈舒颗粒中天麻素和桂皮醛含量测定的方法。方法采用高效液相色谱法,色谱柱：Platisil ODS 柱（4．6mm ×250mm,5μm）,流动相：乙腈（A）－水（B）;梯度洗脱;流速1．0mL? min －1;柱温30℃;检测波长：天麻素为220nm,桂皮醛为290nm;进样量：10μL。结果天麻素和桂皮醛分别在在10．32～206．40μg? mL －1（r ＝0．9998,n＝6）、8．97～179．40μg? mL －1（r ＝0．9999,n＝6）范围内与其峰面积呈良好的线性关系。天麻素和桂皮醛的平均加样回收率分别为为100．79％、99．10％,RSD分别为1．32％、1．36％（ n＝6）。结论该方法操作准确、简便、重现性好,可用于颈舒颗粒中天麻素和桂皮醛的含量测定。     

HPLC法测定注射用阿奇霉素的含量

目的：建立反相高效液相法测定注射用阿奇霉素含量的方法。方法采用Inertsil ODS柱（4．6 mm ×250 mm,5μm）,以0．1 mol·L－1乙酸铵（用氨水调节pH值至8．6）—乙腈—甲醇（50∶30∶20）为流动相,流速1．0 mL·min－1,检测波长218 nm,柱温60℃。结果阿奇霉素的线性范围为100～2000 mg·L－1,r＝0．9998,平均回收率98．8％,RSD＝0．6％（n＝9）。结论该方法简便快速、准确,更适于控制注射用阿奇霉素的质量。     

胞磷胆碱钠及其注射液的HPLC测定

建立了测定胞磷胆碱钠和有关物质的HPLC法。采用阴离子交换柱（Partisil-5 SAX柱），0．05mol/L磷酸盐缓冲液（pH3．2－3．4）为流动相，流速1．0ml/min，检测波长为280nm。胞磷胆碱钠在20－250μg/ml浓度范围内，线性良好，r＝0．9991；平均回收率为100．2％。胞磷胆碱钠、胞嘧啶核苷、尿嘧啶核苷、5′－磷酸胞苷、磷酸胞苷－酰替吗啉－DDC、5′－磷酸尿苷和5′－尿苷二磷酸胆碱酯的日内与日间精密度均小于2．0％；最低检测限为0．1－5．2ng。     

HPLC法测定玉叶清火片中3种成分的含量

目的：建立HPLC法测定玉叶清火片中栀子苷、穿心莲内酯和脱水穿心莲内酯的含量。方法采用 Agilent ZORBAX C18色谱柱（4．6×250mm,5μm）;流动相为甲醇－0．2％磷酸水溶液,梯度洗脱;速为1．0mL? min －1;波长切换时间序列采样：0～10min 为238nm;10～22min 为225nm;22～35min为254nm。结果栀子苷进样量在0．122～2．206μg线性关系良好（r＝0．9999,n＝6）,平均回收率为99．76％,RSD为1．1％（n＝9）;穿心莲内酯进样量在0．036～0．652μg线性关系良好（r＝0．9998,n＝6）,平均回收率为100．49％,RSD为1．4％（n＝9）;脱水穿心莲内酯进样量在0．093～1．673μg线性关系良好（r＝0．9999,n＝6）,平均回收率为99．55％,RSD为1．3％（n＝9）。结论该方法简便、快捷、准确,可用于该制剂的质量控制。     

反相离子对高效液相色谱法测定首乌喘息灵胶囊中扑尔敏的含量

本文用反相离子对HPLC法测定首乌喘息灵胶囊中扑尔敏的含量。用十八烷基硅烷键合硅胶为填料；乙腈-水（含0．05mol／LKH2PO4，0．005mol／LPIC－B6，0．2％三乙胺，H3PO4调pH3．0）（40：60）为流动相；流速为1．0ml／min；柱温为室温；检测波长为260nm；线性范围在1～10μg之间，γ=0．9999；精密度RSD（n＝5）为1．27％；重现性RSD（n＝5）为4．82％；平均回收率96．96％，RSD（n＝5）为2．85％；样品在碱性条件下用正已烷提取后进样。     

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.