HPLC 法同时测定陈香露白露片中7个成分的含量

目的 构建同步测定陈香露白露片中甘草苷、甘草酸铵、橙皮苷、川陈皮素、橘皮素、木香烃内酯和去氢木香内酯含量的HPLC法。方法 采用ZORBAX Eclipse XDB-C₁₈色谱柱（4.6 mm×250 mm,5 μm）,流动相为甲醇-0.1%磷酸溶液,梯度洗脱,流速1.0 ml/min,柱温35 ℃,检测波长237 nm（检测甘草苷、甘草酸铵、木香烃内酯、去氢木香内酯）、283 nm（检测橙皮苷）、330 nm（检测川陈皮素、橘皮素）,进样量10 μl,对采集的16批次样品进行7种成分的含量检测。结果 甘草苷、橙皮苷、甘草酸铵、川陈皮素、橘皮素、木香烃内酯、去氢木香内酯的线性范围分别为1.110~55.72（r=0.9992）、22.15~1108（r=0.9995）、6.140~307.2（r=0.9995）、1.130~56.25（r=0.9997）、0.3700~18.75（r=0.9982）、0.5200~26.01（r=0.9991）、1.180~58.95（r=0.9999）μg/ml。回收率（n=9）分别为98.71%、98.12%、98.44%、98.22%、99.17%、99.18%、97.93%,RSD分别为0.16%、0.67%、0.57 %、0.62%、0.48%、0.56%、0.58%。16批样品中甘草苷、甘草酸铵、橙皮苷、川陈皮素、橘皮素、木香烃内酯、去氢木香内酯的含量分别为0.1250~1.174、2.354~7.426、1.822~27.21、0.0370~1.399、0.0723~0.4433、0.0140~0.1990、0.2207~1.407 mg/g。结论 该方法准确性高、重复性好、耐用性强,可用于陈香露白露片的质量控制和评价。     

用HPLC法同时测定自制复方特比萘酚软膏中3个主药成分的含量

目的 建立同时测定自制复方特比萘酚软膏中3个主药成分含量的HPLC法。方法 色谱柱为ZORBAX SB-C₈柱（4.6 mm×250 mm,5 μm）,流动相为甲醇-0.1%磷酸溶液（70∶30）,柱温：30 ℃,流速：1.0 ml/min,检测波长：248 nm,进样量：10 μl。结果 盐酸特比萘芬在20.4～204.0 μg/ml（r =0.999 7）,莫匹罗星在40.4～404.0 μg/ml（r=0.9998）,糠酸莫米松在2.02～20.20 μg/ml（r=0.999 7）的浓度范围呈良好的线性关系,加样回收率分别为99.39%、99.21%、99.97%,RSD分别为0.82%、0.59%、0.81%（n=9）。结论 该方法的专属性、重复性良好,可用于自制复方特比萘酚软膏中的特比萘酚、莫匹罗星、糠酸莫米松的含量测定。     

景天止痛膏质量标准研究

目的 修订景天止痛膏质量标准中的测定方法。方法 采用薄层色谱法（TLC）对当归、川芎、元胡、三七总皂苷进行定性鉴别,应用高效液相色谱法（HPLC）测定制剂中三七皂苷R₁、人参皂苷Rg₁、人参皂苷Rb₁的含量。结果 TLC法鉴别专属性强,分离度好;三七皂苷R₁在0.1604～2.0050μg (r=0.999)、人参皂苷Rg₁在0.8003～10.0035μg (r=1.000)、人参皂苷Rb₁在0.6182～7.7275μg (r=1.000) 范围内呈良好的线性关系,加样回收率分别为101. 43% 、98.75% 、100. 95% ,相对标准偏差（RSD）分别为2.56% 、2.71% 、2.75%。结论 本方法准确可靠、灵敏度高,可用于景天止痛膏的质量控制。     

SPE-HPLC测定风湿骨痛片中6种生物碱类物质的含量

目的 建立SPE-HPLC同时检测风湿骨痛片中6种生物碱类物质含量的方法。方法 采用Welch XB-C₁₈（4.6 mm×250 mm,5 μm）色谱柱,以含乙腈-四氢呋喃（25：15）溶液为流动相A,以0.05%醋酸铵溶液为流动相B进行梯度洗脱,流速为1.0 mL·min^-1,检测波长为235 nm,柱温为30℃,进样量为10 μL。结果 6种生物碱在优化条件下均可有效分离,苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、次乌头碱和乌头碱分别在162.4~8 121 ng（r=1.000 0）、24.96~1 248 ng（r=1.000 0）、58.03~2 902 ng（r=1.000 0）、17.26~863.0 ng（r=1.000 0）、20.16~1 008 ng（r=1.000 0）和19.90~995.0 ng（r=1.000 0）内有良好的线性关系,平均回收率为88%~98%,RSD为1.8%~2.4%。结论 该方法准确、可靠,适用于风湿骨痛片中生物碱类物质含量的分析。     

GC-MS法定性定量分析贴敷类医疗器械中樟脑、薄荷脑、冰片

摘 要 目的:利用气相色谱-质谱联用仪（GC-MS）建立贴敷类医疗器械中樟脑、薄荷脑、冰片的定性和定量分析方法。方法: 采用Agilent HP-INNOWax (30 m×0.25 mm,0.25 μm)毛细管色谱柱;以氦气为载气,流量为1.0 ml·min^-1;柱温80℃维持2 min,以10℃·min^-1的升温速率升至120℃,维持12 min,再以30℃·min^-1的升温速率升至200℃,维持3 min;离子源为电子轰击电离（EI）源,采集模式为全扫描/选择离子检测。结果:能检测出样品中是否添加樟脑、薄荷脑、冰片,并对其进行定量。3种化合物的线性范围分别为1.742～2.177×10³(r=0.998 9),1.982～2.478×10³(r=0.998 9),1.999～2.499×10³ μg·ml^-1(r=0.999 8),线性关系均良好;平均回收率分别为93.3%,98.8%,94.9%(n=9)。结论:方法简便、灵敏、准确、快速,可用于贴敷类医疗器械中樟脑、薄荷脑、冰片的定性和定量检测。     

HPLC同时测定不同产地番石榴叶药材中4种黄酮类成分含量

目的 建立同时测定不同产地番石榴叶药材中金丝桃苷、槲皮素-3-O-β-D-吡喃阿拉伯糖苷、槲皮素-3-O-α-L-呋喃阿拉伯糖苷、槲皮素含量的方法。方法 采用色谱柱为Agilent Eclipse XDB-C₁₈（4.6 mm×250 mm,5 μm）,流动相为甲醇-0.2%磷酸水（梯度洗脱）,流速为1 mL·min^-1,柱温为35℃,检测波长为360 nm,进样量10µL。结果 金丝桃苷、槲皮素-3-O-β-D-吡喃阿拉伯糖苷、槲皮素-3-O-α-L-呋喃阿拉伯糖苷、槲皮素检测进样量线性范围分别为0.155~3.100 μg （r=1.000 0）,0.159~3.182 μg （r=0.999 8）,0.180~3.601 μg （r=0.999 8）,0.007~0.135 μg （r=1.000 0）;精密度,稳定性,重复性试验的RSD<2.0%;加样回收率分别为100.32%（RSD=1.44%,n=6）,97.79%（RSD=1.11%,n=6）,100.73%（RSD=1.43%,n=6）,98.33%（RSD=1.48%,n=6）,10批不同产地的番石榴叶药材中4种黄酮类成分含量差异较大。结论 该方法简便、专属性强、准确度高、重复性好,可用于不同产地番石榴叶药材的质量控制。     

HPLC双波长法测定复方罗布麻片Ⅰ中泛酸钙和氢氯噻嗪的含量

目的 建立HPLC双波长法测定复方罗布麻片Ⅰ中泛酸钙和氢氯噻嗪的含量。方法 采用Kromasil C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以含0.1%辛烷磺酸钠溶液（用磷酸调节pH值至3.0）-乙腈（96：4）为流动相A,以甲醇为流动相B,采用梯度洗脱,柱温为35℃,检测波长泛酸钙200 nm、氢氯噻嗪275 nm,流速为1.0 mL·min^-1,进样量为10 μL。结果 泛酸钙和氢氯噻嗪分别在0.025~0.5 μg（r=0.999 6）和0.16~3.2 μg（r=1.000 0）内线性关系良好;平均加样回收率（n=9）分别为101.2%（RSD=0.47%）和101.6%（RSD=0.49%）。结论 本法精密度好,结果准确可靠,适用于该制剂的质量检验分析。     

HPLC法测定肝素钠注射液中6种抑菌剂

目的 建立高效液相色谱（HPLC）法同时测定肝素钠注射液中苯酚、苯甲醇、三氯叔丁醇、羟苯甲酯、羟苯乙酯、羟苯丙酯6种抑菌剂。方法 采用Agilent Zorbax SB-C₁₈（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,检测波长为220 nm及256 nm,柱温30 ℃。结果 苯酚、苯甲醇、羟苯甲酯、羟苯乙酯、三氯叔丁醇、羟苯丙酯分别在25.00~400.06 μg·mL^-1（r=1.000 0）、104.49~1 671.88 μg·mL^-1（r=0.999 9）、30.65~490.4 μg·mL^-1（r=0.999 9）、5.36~85.81 μg·mL^-1（r=0.999 9）、49.60~793.54 μg·mL^-1（r=0.999 9）、5.03~80.45 μg·mL^-1（r=1.000 0）内线性关系良好,平均回收率分别为100.3%、99.7%、99.8%、100.0%、99.4%和100.1%,RSD分别为1.0%、1.2%、1.3%、1.4%、1.4%和1.4%（n=9）。结论 方法准确,重现性好,结果可靠,可用于肝素钠注射液中6种抑菌剂的测定。     

玄膝荣筋散质量标准研究

目的 修订玄膝荣筋散的定性和定量测定方法。方法 采用薄层色谱（TLC）法对川芎、穿山龙进行定性鉴别,HPLC法测定制剂中桂皮醛的含量。采用KR100-5C₁₈ 色谱柱(250mm×4.6mm,5μm),流动相为乙腈-水（35∶65）,检测波长为290 nm。结果 TLC法能定性鉴别川芎、穿山龙。桂皮醛在0.0489~0.3260μg/ml范围内线性关系良好（r=1.00）。平均加样回收率为95.71%（RSD=1.78%）。结论 该法灵敏度高、专属性好、操作简便、重现性好。     

气相色谱法测定复方樟脑搽剂中樟脑与薄荷脑含量及其不确定度评估

目的 建立测定复方樟脑搽剂中主要成分樟脑和薄荷脑含量的气相色谱（GC）法,并探讨不确定度评估方法。方法 采用GC法,以萘为内标物,Thermo TG-WAXMS毛细管柱（30.0 m×0.25 mm,涂层厚0.5 μm）,FID检测器;分析测量过程不确定度的来源,建立数学模型,计算合成标准不确定度和扩展不确定度。结果 樟脑和薄荷脑分别在8.56~85.6μg/ml、11.2~112.0 μg/ml质量浓度范围内线性关系良好,樟脑平均加样回收率100.20%、RSD为0.892%（n=9）,薄荷脑平均加样回收率99.65%、RSD为1.369%（n=9）;扩展不确定度分别为0.630 mg/ml （k=2）、0.656 mg/ml （k=2）,樟脑含量为（20.74±0.630） mg/ml、薄荷脑含量为（20.48±0.656） mg/ml。结论 气相色谱方法准确、灵敏、重现性好,可用于复方樟脑搽剂中樟脑和薄荷脑含量测定;不确定度评定有利于进一步提高含量测定的准确性。     

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.     

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.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

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.     

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.