HPLC法测定注射用七叶皂苷钠中七叶皂苷A和B的含量

目的:建立高效液相色谱法测定七叶皂苷钠中七叶皂苷 A 和 B 的含量。方法:反相高效液相色谱法,色谱柱为 ZORB-AX Eclipse XDB-C_(18)(4.6mm×150 mm,5μm)(美国 Agilent 公司生产),乙腈-磷酸(取85%磷酸5.5 mL,用水稀释至1000mL)(33:67)为流动相,流速为1.0 mL·min~(-1),检测波长为220 nm,用外标法定量。结果:七叶皂苷 A 在170～1510μg·mL~(-1)范围内有良好的线性关系,r=0.9999,其低、中、高3个量回收率的平均值分别为98.5%,102.8%和103.4%;RSD 分别为1.9%,1.3%和1.2%。七叶皂苷 B 在120～1110μg·mL~(-1)范围内有良好线性关系,r=0。9999,其低、中、高3个量回收率的平均值分别为99.2%,102.4%和102.6%;RSD 分别为0.9%,1.1%和1.0%。结论:本方法可测定叶皂苷钠中七叶皂苷 A和 B 的含量,且可靠、简便。     

紫外分光光度法测定七叶皂苷钠含量

目的:建立紫外分光光度法测定七叶皂苷钠含量.方法:用紫外分光光法测定七叶皂苷钠的含量,并将测定的方法与滴定法进行比较.结果:七叶皂苷钠在30～150 mg·L-1浓度范围内,吸收度与浓度线性关系良好(r=0.999 4).其回收率为99.63%,RSD为0.52%(n=9).结论:本法简便、快速,可用于七叶皂苷钠含量测定.     

反相高效液相色谱法测定苯酰甲硝唑有关物质

目的:建立反相高效液相色谱法测定苯酰甲硝唑有关物质。方法:采用双波长检测,梯度洗脱。色谱柱为迪马公司 Dia-monsil~(TM)C_(18)(250mm×4.6mm,5μm);流动相 A 和 B 分别为1.5g·L~(-1)磷酸二氢钾溶液(用1mol·L~(-1)磷酸溶液调 pH3.2)-乙腈(80:20和58:42);流速1.0mL·min~(-1),检测波长为235,315nm,进样量20μL,柱温为室温,外标法和主成分自身对照法计算。结果:杂质 A、杂质 B、杂质 C、苯酰甲硝唑均能达到很好的分离,并分别在1.12～16.8μg·mL~(-1)(r=1.000),1.12～16.8μg·mL~(-1)(r=0.9999),1.0～15.0μg·mL~(-1)(r=1.000),1.04～15.6μg·mL~(-1)(r=0.9992)浓度范围内具有良好的线性关系。杂质 A、杂质 B、杂质 C 的平均回收率(n=9)分别为99.4%,99.6%,99.5%。结论:本法简便、灵敏、准确,专属性强,适合于苯酰甲硝唑有关物质的测定。     

高效液相色谱法同时测定注射用丹红（粉针剂）中4种有效成分

目的:同时测定注射用丹红(粉针剂)中丹参素、原儿茶醛、羟基红花黄色素 A 和丹酚酸 B 的含量。方法:采用高效液相色谱法,色谱柱:Luna C_(18)柱(250 mm×4.6 mm,5μm);流动相:0.05%磷酸水溶液(A)-乙腈(B),梯度洗脱程序为:0～80min,A:100%→67%,B:0%→33%;流速:1.0 mL·min~(-1);检测波长:280 nm。结果:建立了同时测定注射用丹红(粉针剂)中4种成分含量的方法。丹参素、原儿茶醛、羟基红花黄色素 A 和丹酚酸 B 的线性范围分别为56.3～338μg·mL~(-1)(r=0.9997),7.92～47.2μg·mL~(-1)(r=0.9996),16.4～98.2μg·mL~(-1)(r=0.9997),32.0～193μg·mL~(-1)(r=0.9999);平均回收率(n=9)分别为99.7%,99.3%,99.2%,98.8%。结论:该方法简便、准确,重复性好,为注射用丹红(粉针剂)的质量控制提供了定量方法。     

褪色分光光度法测定七叶皂苷钠

目的:建立褪色分光光度法测定七叶皂苷钠。方法:在 pH 3.5～4.2的 Britton—Robinson 缓冲溶液中,七叶皂苷钠与夜蓝反应,形成离子缔合物时能使染料发生明显的褪色作用。产生最大褪色波长为614 nm,并且吸收度降低与七叶皂苷钠浓度成正比。结果:七叶皂苷钠浓度在0.25～20.0μg·mL~(-1)范围内符合比耳定律,摩尔吸光系数为1.4×10~4L·mol~(-1)·cm~(-1),方法具有较高的灵敏度,其检出限为75 ng·mL~(-1),研究了共存物质的影响,表明方法选择性好。结论:此法简便、准确、灵敏,可用于片剂和尿样中七叶皂苷钠的测定。     

高效液相色谱法同时测定白带净丸中的3'-羟基葛根素、葛根素、尿囊素、川续断皂苷Ⅵ和茯苓酸的含量

目的建立同时测定白带净丸中3'-羟基葛根素、葛根素、尿囊素、川续断皂苷Ⅵ和茯苓酸的HPLC法。方法采用Dikma-C_(18)(250 mm×4.6 mm,5μm),以乙腈(A)-0.5%磷酸溶液(B)为流动相,梯度洗脱,流速0.9 mL·min~(-1),柱温30℃,进样量为10μL。结果 3'-羟基葛根素、葛根素、尿囊素、川续断皂苷Ⅵ和茯苓酸的线性范围分别为:6.14~122.80μg·mL~(-1)(r=0.9993),7.59~151.80μg·mL~(-1)(r=0.9991),4.15~83.00μg·mL~(-1)(r=0.9999),8.13~162.60μg·mL~(-1)(r=0.9994),5.35~107.00μg·mL~(-1)(r=0.9997);平均回收率及RSD均符合药典规定。结论所建方法重复性好,专属性强,可用于白带净丸的质量控制。     

注射用七叶皂苷钠在健康人体的药代动力学

目的 研究健康志愿者单剂量静脉滴注七叶皂苷钠(扩张血管中药)后的药代动力学.方法 9名健康男性志愿者单剂量静脉滴注七叶皂苷钠10 mg后,用高效液相色谱法-串联质谱法测定血浆和尿液中七叶皂苷A、B 2组分浓度,用WinNonLin 5.0计算主要药代动力学参数.结果 健康志愿者单剂量静脉滴注七叶皂苷钠10 mg后,七叶皂苷中A、B 2组分的主要药代动力学参数:Cmax分别为(283.00±70.53)、(206.33±57.20)ng·mL~(-1);AUC_(0-t)分别为(1008.05±396.49)、(638.96 4-259.48)ng·mL~(-1)·h;t_(1/2)分别为(3.72±0.44)、(3.57±0.48)h;Vz分别为(19.39±7.05)、(23.82±11.43)L;CL分别为(3.66±1.36)、(4.55±1.86)L·h~(-1);36 h尿累积排泄百分率分别为(4.91±1.38)%、(2.80±0.71)%.结论 健康人体对七叶皂苷中A、B 2组分的处置过程大致相同,消除半衰期约3.6 h,原形药物尿排泄百分率较低.     

HPLC法同时测定肿痛安胶囊中5种成分的含量

目的建立同时测定肿痛安胶囊中:天麻素、升麻素苷、5-O-甲基维斯阿米醇苷、欧前胡素和异欧前胡素含量的HPLC法。方法色谱柱:Phenomenex Luna C_(18)柱(250mm×4.6mm,5μm);流速:1.0mL·min~(-1);柱温:25℃;流动相:甲醇-水梯度洗脱;检测波长:230nm;进样量:5μL。结果天麻素质量浓度在12.46～199.30μg·mL~(-1)范围内线性关系良好,r_1=0.999 5,平均回收率为101.2%,RSD值为1.6%(n=6);升麻素苷质量浓度在12.07～193.20μg·mL~(-1)范围内线性关系良好,r_2=0.999 7,平均回收率为100.1%,RSD值为1.8%(n=6);5-O-甲基维斯阿米醇苷质量浓度在8.12～129.90μg·mL~(-1)范围内线性关系良好,r_3=0.999 8,平均回收率为99.1%,RSD值为1.7%(n=6);欧前胡素质量浓度在12.52～200.40μg·mL~(-1)范围内线性关系良好,r_4=0.999 6,平均回收率为98.6%,RSD值为1.4%(n=6);异欧前胡素质量浓度在12.65～202.40μg·mL~(-1)范围内线性关系良好,r_5=0.999 6,平均回收率为99.0%,RSD值为0.7%(n=6)。结论该方法简单、准确,可同时测定5种成分的含量,可用于肿痛安胶囊的质量控制。     

新复方大青叶片中4种西药成分的含量测定方法的研究

目的:建立新复方大青叶片中扑热息痛、咖啡因、异戊巴比妥和维生素 C 的含量测定方法。方法:采用 HPLC 法测定了扑热息痛、咖啡因、异戊巴比妥和维生素 C 的含量。结果:扑热息痛在199.5～1247μg·mL~(-1)范围内呈良好的线性关系(r=0.9998),平均回收率为99.81%,RSD=0.99%(n=6);咖啡因在20.64～129μg·mL~(-1)范围内呈良好的线性关系(r=0.9999),平均回收率为100.8%,RSD=1.43%(n=6);异戊巴比妥在8.42～210.5μg·mL~(-1)范围内呈良好的线性关系(r=0.9998),平均回收率为100.4%,RSD=1.41%(n=6);维生素 C 在40.48～253.0μg·mL~(-1)范围内呈良好的线性关系(r=0.9999),平均回收率为99.36%,RSD=1.42%(n=6)。结论:含量测定方法简便准确,重复性好,可用于控制新复方大青叶片的质量。     

高效液相色谱法及分光光度法测定黄姜中皂苷的含量

目的:建立测定陕西不同产地黄姜中皂苷含量的方法。方法:利用高效液相色谱法测定黄姜中黄姜素 A 的含量,色谱件为 HiQsil C_(18)柱(250 mm×4.6 mm,10μm),流动相为乙睛-水(45:55),流速为1 mL·min~(-1),柱温为室温;Alltech 蒸发光散射检测器参数:载气为氮气,流速2.5 L·min~(-1),漂移管温度90℃,压力0.45 MPa;采用分光光度法测定黄姜中总皂苷的含量,以对二甲氨基苯甲醛为显色剂,测定波长为518 mm。结果:HPLC 法测定,黄姜素 A 进样量在0.40～4.02μg范围内有良好线性关系(r=0.9991);黄姜素 A 的平均回收率(n=6)为103.2%,RSD 为1.6%。用分光光度法测定,线性范围4.4～55μg·mL~(-1)(r=0.9992);总皂苷平均回收率(n=3)为99.1%,RSD 为1.8%。结论:本文的2种方法快速简便,结果准确可靠,重复性好,均可用于对黄姜药材进行质量控制。     

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.     

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.