高效液相色谱法测定盐酸苯海拉明注射液中苯甲醇含量

目的 采用高效液相色谱法建立测定盐酸苯海拉明注射液中苯甲醇的方法.方法 色谱柱Agilent氰基柱（250mm×4.6mm,5μm）,流动相为乙腈-20mM乙酸铵（用甲酸调pH值至6.5）（50：50）,检测波长为257nm.结果 苯甲醇浓度在0.625～3.75μL·mL-1范围内与峰面积呈良好的线性关系,r为1.000;苯甲醇加样回收率的平均值为100.3%,RSD=1.4%.结论 本方法简便、准确可靠,适用于盐酸苯海拉明注射液中苯甲醇的质量控制.     

HPLC法测定妥布霉素滴眼液中5种抑菌剂

目的 建立同时测定妥布霉素滴眼液中5种抑菌剂(羟苯乙酯、硫柳汞、羟苯丙酯、苯扎溴铵和苯扎氯铵)的HPLC方法。方法 采用Agilent Zorbax SB-C₁₈ (4.6 mm×150 mm,5 μm)色谱柱,流动相A为1%三乙胺（磷酸调节pH值至3.5±0.05）;流动相B为甲醇,梯度洗脱,流速为1.0 mL·min^-1,柱温35 ℃,检测波长为214 nm。结果 羟苯乙酯、硫柳汞、羟苯丙酯、苯扎溴铵/苯扎氯铵各峰均分离良好;羟苯乙酯在0.77～192.5 μg·mL-1范围内线性关系良好(r=0.999 5),平均回收率为100.0%(RSD=0.9%,n=9);硫柳汞在2.16～541.0 μg·mL^-1范围内线性关系良好(r=0.999 7),平均回收率为100.1%(RSD=0.6%,n=9);羟苯丙酯在0.84～209.8 μg·mL^-1范围内线性关系良好(r=1.000 0),平均回收率为100.3%(RSD=1.0%,n=9);苯扎溴铵在4.36～1090 μg·mL^-1范围内线性关系良好(r=0.9992),平均回收率为100.2%(RSD=0.5%,n=9);苯扎氯铵（n-C12H25）3.22～805.0 μg·mL^-1范围内线性关系良好(r=0.999 8),平均回收率为100.1%(RSD=1.1%,n=9);苯扎氯铵（n-C14H29）1.66～413.9 μg·mL^-1范围内线性关系良好(r=1.000 0),平均回收率为100.1%(RSD=0.6%,n=9)。结论 该方法准确、灵敏、简便,可用于妥布霉素滴眼液中羟苯乙酯、硫柳汞、羟丙丙酯、苯扎溴铵及苯扎氯铵5种抑菌剂的检查。     

HPLC同时测定黄石感冒片中阿魏酸、芦丁、大黄酸、大黄素和大黄酚的含量

目的 建立HPLC同时测定黄石感冒片中阿魏酸、芦丁、大黄酸、大黄素和大黄酚的含量。方法 采用HPLC,色谱柱为Welch Topsil-C₁₈柱(4.6 mm×250 mm,4 μm);以甲醇-0.1%磷酸溶液(78∶22)为流动相;流速：1.0 mL·min^-1;柱温：30 ℃;检测波长：280 nm。结果 阿魏酸、芦丁、大黄酸、大黄素和大黄酚峰线性范围分别为0.020 82~0.416 3 μg·mL^-1(r=0.999 7),0.011 32~0.278 3 μg·mL^-1(r=0.999 3),0.017 22~0.344 3 μg·mL^-1(r=0.999 5),0.015 79~0.315 8 μg·mL^-1(r=0.999 6)和0.051 34~1.027 μg·mL^-1(r=0.999 9),平均加样回收率分别为97.4%(RSD=1.1%),95.0%(RSD=0.88%),97.5%(RSD=1.3%),97.4%(RSD=1.4%)和96.3%(RSD=0.87%)。结论 新建方法简便、准确,可用于黄石感冒片的定量分析方法。     

HPLC法测定布洛伪麻缓释片的释放量

摘 要 目的:建立高效液相色谱法测定布洛伪麻缓释片释放量的方法。方法: 色谱柱为迪马 C₁₈（250 mm×4.6 mm,5 μm）,流动相为甲醇-三乙胺-0.04 mol·L^-1 磷酸二氢钠溶液 (60∶0.02∶40),流速为1.0 ml·min^-1,检测波长为215 nm,柱温为35℃,进样量为20 μl。结果:布洛芬的线性范围为40～2 000 μg·mL^-1（r＝1.000 0）,平均加样回收率为99.2％,RSD＝0.8％(n=9),最低定量浓度为0.04μg· mL^-1;盐酸伪麻黄碱的线性范围为6～300 μg·mL^-1（r＝1.000 0）,平均加样回收率为98.5％,RSD＝0.6％(n=9),最低定量浓度为0.06μg· mL^-1。结论: 该方法简便快速、准确灵敏,可用于布洛伪麻缓释片释放量的测定。     

HPLC法检测醋酸奥曲肽注射剂中5种抑菌剂

目的：检测醋酸奥曲肽注射剂中是否添加苯酚、苯甲醇、三氯叔丁醇、对羟基苯甲酸甲酯及对羟基苯甲酸丙酯5种抑菌剂。方法：采用C18（L）（4.6 mm×250 mm,5 μm）色谱柱,流动相A为水,流动相B为甲醇,梯度洗脱,流速为1.0 mL·min^-1,柱温30℃,检测波长为220 nm及256 nm。结果：苯酚、苯甲醇、三氯叔丁醇、对羟基苯甲酸甲酯及对羟基苯甲酸丙酯各峰均分离良好;苯酚在1.29~258.60 μg·mL^-1范围内线性关系良好（r=1.000）,平均回收率为100.0%（n=9）;苯甲醇在2.72~544.20 μg·mL^-1范围内线性关系良好（r=0.9997）,平均回收率为100.3%（n=9）;三氯叔丁醇在9.95~1990.00 μg·mL^-1范围内线性关系良好（r=1.000）,平均回收率为100.9%（n=9）;对羟基苯甲酸甲酯在0.27~53.80 μg·mL^-1范围内线性关系良好（r=1.000）,平均回收率为100.5%（n=9）;对羟基苯甲酸丙酯在0.26~52.00 μg·mL^-1范围内线性关系良好（r=1.000）,平均回收率为99.4%（n=9）;91批醋酸奥曲肽注射剂中均未检出5种抑菌剂。结论：该方法准确、灵敏、简便,可用于醋酸奥曲肽注射剂中苯酚、苯甲醇、三氯叔丁醇、对羟基苯甲酸甲酯及对羟基苯甲酸丙酯5种抑菌剂的检查。     

HPLC法测定盐酸艾司洛尔注射液含量的改进

摘 要 目的：改进盐酸艾司洛尔注射液含量测定的HPLC方法。方法: 采用HPLC法,色谱柱为Welch Xltimate C18柱（250 mm×4.6 mm,5 μm）,流动相为乙腈 甲醇 磷酸盐缓冲液（15∶20∶65）,检测波长为222 nm,流速为1.0 ml·min^-1,柱温为30℃,进样体积为20 μl。结果:盐酸艾司洛尔的浓度范围在12.26～196.16 μg·mL^-1时,峰面积与浓度呈良好的线性关系（r=1.000 0）;平均回收率为101.2%（RSD=0.7%,n=9）。结论:建立的盐酸艾司洛尔注射液HPLC简便、快速、准确、专属性强,比现行标准更能反应药物含量的真实水平,更适用于盐酸艾司洛尔注射液的含量测定。     

西红花酸在大鼠的药代动力学研究

目的建立高效液相色谱法测定大鼠血浆中西红花酸的浓度。方法用HPLC法,色谱柱为Hypersil C₁₈柱(5 μm,4.6 mm×200 mm),流动相为甲醇-水-冰醋酸(75∶24.5∶0.5),流速1.0 mL·min^-1,柱温30℃,检测波长423 nm。结果西红花酸浓度0.49～7.87 μg·mL^-1与峰面积呈良好的线性关系(γ=0.9996),最低检测浓度为0.14 μg·mL^-1(S/N=3)。样品的平均加样回收率为105.2%。日内、日间精密度的RSD均小于5%。不同时间、不同温度及冻融处理的稳定性考察,RSD分别为7.4%,4.9%和3.3%。结论本法稳定、简单、可靠,可用于西红花酸血药浓度分析及其药代动力学研究。     

HPLC同时测定冠心康颗粒中芍药苷、丹酚酸B和羟基红花黄色素A的含量

目的 建立同时测定冠心康颗粒中芍药苷、丹酚酸B和羟基红花黄色素A含量的方法。方法 采用Welchrom C₁₈色谱柱(250 mm×4.6 mm,5 μm),以乙腈(A)-0.1%磷酸(B)为流动相,梯度洗脱;流速：1.0 mL·min^-1;检测波长：230 nm。结果 芍药苷在7.02~52.64 μg·mL^-1内呈良好的线性关系(r=0.999 7),平均回收率为99.3%,RSD为1.2%;丹酚酸B在23.19~173.90 μg·mL^-1内呈良好的线性关系(r=0.999 7),平均回收率为98.2%,RSD为1.1%;羟基红花黄色素A在4.47~ 33.50 μg·mL^-1内呈良好的线性关系(r=0.999 3),平均回收率为98.0%,RSD为1.0%。结论 本法简便、灵敏、准确、重复性好,可用于冠心康颗粒的质量控制。     

苯扎贝特纳米脂质载体的包封率测定

目的 建立苯扎贝特纳米脂质载体包封率的测定方法。方法 采用葡聚糖凝胶柱层析法分离苯扎贝特纳米脂质载体中的游离药物,高效液相色谱法测定其含量,计算包封率。色谱条件：采用Agilent ZORBAX SB-C₁₈柱(250 mm×4.6 mm,5 μm),流动相为0.01 mol·L^-1磷酸盐缓冲液(pH 3.0)-甲醇(30∶70),流速：1.0 mL·min^-1,检测波长：230 nm,进样量：20 μL。结果 苯扎贝特峰与杂质峰的分离度良好,苯扎贝特浓度在4.44~177.6 μg·mL^-1内与峰面积呈良好的线性关系(r=0.999 9),平均回收率为99.23%(RSD=0.68%)。3批苯扎贝特纳米脂质载体的包封率均>75%。结论 本方法简便、准确,灵敏度高,可用于苯扎贝特纳米脂质载体的质量控制。     

HPLC测定达比加群酯中的有关物质

目的 建立达比加群酯原料药中有关物质的测定方法。方法 采用Agilent SB-C₁₈色谱柱(250 mm×4.6 mm,5 μm),以乙腈(A)-0.2%的醋酸铵(B,用冰醋酸调节pH值至4.4)为流动相进行梯度洗脱：0~18 min,90%→40%B;18~30 min,40%B。流速为1.0 mL·min^-1,检测波长为340 nm。结果 各杂质与主峰之间的分离度良好。5个已知杂质：杂质A浓度在0.117 0~1.872 μg·mL^-1内与峰面积呈良好的线性关系,r为0.999 7;杂质B浓度在0.126 5~2.024 μg·mL^-1内与峰面积呈良好的线性关系,r为0.999 5;杂质C浓度在0.113 0~1.808 μg·mL^-1内与峰面积呈良好的线性关系,r为0.999 5;杂质D浓度在0.120 5~1.928 μg·mL^-1内与峰面积呈良好的线性关系,r为0.999 9;杂质E浓度在0.123 0~1.968 μg·mL^-1内与峰面积呈良好的线性关系,r为0.999 6;杂质A、杂质B、杂质C、杂质D和杂质E加样回收率的平均值分别为98.75%,98.91%,98.39%,99.0%和99.73%;RSD分别为0.91%,1.09%,1.22%,1.35%和1.18%。结论 本方法简便、准确可靠,适用于达比加群酯中有关物质的控制。     

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.     

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.