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1.
中药和保健食品中非法添加降脂类药物的检测方法研究 总被引:3,自引:0,他引:3
目的:建立准确、灵敏的HPLC—MS/MS方法检查中药制剂及保健品中非法添加的10种化学降酯药物(烟酸、普伐他汀钠、瑞舒伐他汀钙、苯扎贝特、阿托伐他汀、氟伐他汀钠、吉非罗齐、洛伐他汀、非诺贝特、辛伐他汀)。方法:用WatersSunfireC18色谱柱(4.6mm×150mm,5μm),梯度洗脱:流动相A为20mmol·L-1醋酸铵溶液,流动相B为甲醇。选择正负离子检测10种临床常用降脂药物,利用质谱解析软件研究了该类化合物的质谱裂解规律,通过比较样品峰与对照品峰的一级质谱、二级质谱质荷比,确定样品中是否掺杂了化学降脂药物。结果:HPLC—MS/MS方法测定上述化学物质不受药物辅形剂干扰,各药物色谱峰之间分离度良好,质谱分别率符合要求,10种降脂药的最小检出量为2ng至40ng。结论:该方法灵敏度、准确性均可满足定性研究的要求,简便、快捷。 相似文献
2.
建立了HPLC/MS/MS测定大鼠血浆中的积雪甙。以柴胡皂甙D为内标,采用XTerra C18柱,流动相为O.1%乙酸和含O.1%乙酸的乙腈,梯度洗脱。质谱条件为电喷雾离子源,检测方式为多反应检测,定量分析离子为m/z981.5→493(积雪甙)和803→331(柴胡皂甙D),血浆样品采用固相萃取处理。检测限为0.5ng/ml。 相似文献
3.
建立了LC—MS/MS法测定丙酸倍氯米松及其代谢产物单丙酸倍氯米松在Beagle犬血浆中的浓度。血浆样品用乙醚萃取,采用Inersil—ODS 3色谱柱,甲醇-水(85:15,含2mmol/L甲酸铵,甲酸调至pH3.6)为流动相,流速0.2ml/min。使用电喷雾离子源接口,可同时检测丙酸倍氯米松和单丙酸倍氯米松。血浆中丙酸倍氯米松的线性范围为0.1~10ng/ml,相对回收率96.0%~104.3%,日内、日间RSD小于11.0%和9.1%。 相似文献
4.
人血浆中奥美沙坦的HPLC-MS/MS测定 总被引:3,自引:0,他引:3
建立了HPLC—MS/MS法测定人血浆中的奥美沙坦,以替米沙坦为内标。采用C18色谱柱,流动相为甲醇-水(64:36,含0.2%乙酸)。质谱条件为电喷雾离子源,多离子反应监测,定量分析离子为m/z447→429(奥美沙坦)和m/z515→497(替米沙坦)。血浆样品采用固相萃取处理,线性范围为4~1000ng/ml,检测限为1ng/ml。 相似文献
5.
几种氟喹诺酮药物含量测定的色谱条件比较及用HPLC法测定依诺沙星制剂的含量 总被引:1,自引:0,他引:1
目的:对中国药典2000年版中收载的四种氟喹诺酮药物的含量测定方法的专属性进行考证,同时给出专属性好的方法,并对依诺沙星各剂型的HPLC法进行定量研究。方法:采用反相HPLC法,以0.01mol/L溴化四丁基铵与0.05mol/L磷酸二氢钾混合溶液(用磷酸调节pH值至2.8)-乙腈(90:10)为流动相;检测波长为278nm。结果:四种氟喹诺酮药物在该流动相中可以有效分离,并可用于依诺沙星及其制剂的定量。结论:可用此流动相系统对四种氟喹诺酮药物进行分离和定量测定。 相似文献
6.
用细胞膜色谱法和HPLC-TOF/MS研究附子中的有效成分 总被引:1,自引:0,他引:1
目的通过细胞膜色谱技术和高效液相-飞行时间质谱(HPLC-TOF/MS)技术相结合,初步筛选和鉴定附子中的有效成分。方法初步筛选采用自制的大鼠心肌细胞膜色谱柱,流动相为10mmol/L磷酸盐缓冲溶液,流速为0.2ml/min。色谱分离采用SHISEIDO CAPCELL PAKC18柱,流动相为0.1%甲酸水溶液和乙腈,梯度洗脱,流速为1.0ml/min。质谱鉴定采用TOF/MS,正离子模式扫描。结果确定了附子中8个可能的有效成分。结论通过细胞膜色谱技术和HPLC-TOF/MS技术相结合,为从天然产物中快速寻找新的活性成分提供了途径。 相似文献
7.
目的建立HPLC-MS/MS法检测中成药及保健品中可能非法添加的10种解热镇痛类化学药物。方法样品经甲醇提取,采用液相色谱-质谱联用法测定。色谱条件:SHIMADZU Shim-packVPODS(250 mm×4.6 mm,5μm)C18色谱柱,梯度洗脱:流动相A为20 mmol.L-1醋酸铵,流动相B为乙腈;质谱条件:电喷雾离子化正、负离子检测方式(ESI+、ESI-),全扫描一级质谱、选择离子二级扫描质谱检测方式,通过与标准谱库中保留时间和多级质谱图的双重对比,对样品中非法添加的解热镇痛类化学药物进行定性鉴别。结果在25批供试品中,检测到有4种样品中含有解热镇痛类化学药物。结论该方法简便、快捷,准确性、灵敏度均可满足定性检查的要求。 相似文献
8.
人血浆中苦参素的HPLC-MS测定 总被引:1,自引:0,他引:1
建立了HPLC—MS法测定人血浆中苦参素浓度,并用于其胶囊的药物动力学研究。以非那雄胺为内标,采用C18柱,流动相为5mmol/L乙酸铵(含0.05%三乙胺)-甲醇(18:82,乙酸调至pH6.2)。质谱条件为电喷雾离子源,选择检测离子为m/z 265.2(苦参素)和m/z 373.3(非那雄胺)。苦参素在2.5~500ng/ml范围内线性关系良好。 相似文献
9.
小分子药物的APCI/MS研究 总被引:2,自引:2,他引:2
目的:建立可用于小分子药物分析的高灵敏大气压化学解离/质谱(APCI/MS)方法。方法:比较电喷雾离子化(ESI)/MS与APCI/MS对58种小分子药物在1μg进样量下的灵敏度,考察其中44种小分子药物在AP-CI/MS条件下的质谱行为;以其中5种小分子药物为模型化合物,观察碰撞诱导解离电压(CID电压)对APCI/MS的影响。结果:在相同的质谱条件下,APCI/MS测定小分子药物的灵敏度明显高于ESI/MS;在APCI/MS条件下,小分子药物的分子离子峰,大多数为基峰,少数为强峰,极少数为弱峰,此外,还给出了丰富的碎片峰,小分子经物的结构与CID电压对APCI/MS的分子离子峰及碎片离子丰度有明确的影响。结论:APCI/MS作为一种高灵敏分析方法在与小分子药物的体内过程相关的研究中有广泛应用前景。μμ 相似文献
10.
建立了高效液相色谱法检查磷酸可待因、磷酸可待因与精氨酸布洛芬复方的有关物质,并采用HPLC-TOF/MS和LC—MS/MS对磷酸可待因及两种复方药物产生的降解产物进行了结构鉴定。色谱柱为ClR(250mm×4.6mm,5μm),柱温50℃,流速1mL/min,检测波长245nm,醋酸铵(0.04M,用醋酸调pH6.0)-乙腈(92:8,v/v)为流动相A,乙腈为流动相B,梯度洗脱。磷酸可待因在氧化条件下很不稳定产生了两个N-氧可待因异构体,在碱性破坏中得到了新的杂质,其结构可能为6-羟基-3-甲氧基-17-甲基-7,8-双脱氢吗啡-5-醇。在酸性破坏条件下磷酸可待因和精氨酸布洛芬可发生酯化反应。所建立的HPLC方法灵敏、准确,可有效测定磷酸可待因、磷酸可待因与精氨酸布洛芬复方的有关物质,并对产生的降解产物进行了结构鉴定,为更好的控制磷酸可待因与磷酸可待因复方药物的质量提供了依据。 相似文献
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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.
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.相似文献
14.
Petrikovics I McGuinn WD Sylvester D Yuzapavik P Jiang J Way JL Papahadjopoulos D Hong K Yin R Cheng TC DeFrank JJ 《Drug delivery》2000,7(2):83-89
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. 相似文献
16.
Chang Min Kim Kun Ho Son Sung Hwan Kim Hyun Pyo Kim 《Archives of pharmacal research》1991,14(4):305-310
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. 相似文献
17.
《Critical reviews in toxicology》2013,43(5-6):327-369
AbstractThe 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. 相似文献
18.
《Expert opinion on investigational drugs》2013,22(1):79-86
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. 相似文献
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