共查询到18条相似文献,搜索用时 172 毫秒
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固相萃取技术是近年来发展较快并得到广泛应用的一种样品前处理方法 (分离、纯化、富集), 具有节省时间、溶剂消耗少, 富集倍数高, 准确度高等优点。随着科学技术的不断发展及研究的不断深入, 多种优于传统固相萃取技术的新型固相萃取新技术如分子印迹固相萃取、磁性固相萃取、固相微萃取等不断出现并广泛应用到食品、药品、生物及环境监测等领域。本文对几种固相萃取新技术的基本原理、方法及近十年来在不同研究领域的研究应用进行综述。 相似文献
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目的:建立鱼腥草注射液顶空固相微萃取-气相色谱-质谱联用分离鉴定及含量测定新方法,通过顶空固相微萃取与传统水蒸气蒸馏、固相萃取等提取工艺比较,为改进鱼腥草注射液制备工艺奠定基础。方法:以色谱峰总面积为指标,对萃取头种类等5项顶空固相微萃取关键提取条件进行优化,分别采用顶空固相微萃取、水蒸气蒸馏、固相萃取等3种方法提取鱼腥草注射液中的挥发性成分,通过分离出色谱峰个数、鉴定出化合物数量、精密度等指标比较提取效果。结果:顶空固相微萃取对鱼腥草注射液中挥发性成分的提取效果最佳。结论:顶空固相微萃取具有操作简便、快捷、不污染环境、精密度高等优点,可用于鱼腥草注射液中挥发性成分提取、分析。 相似文献
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固相萃取-毛细管气相色谱法测定莪术中15种有机氯农药的残留量 总被引:1,自引:1,他引:1
目的用固相萃取-毛细管气相色谱分析方法测定莪术中15种有机氯农药残留量。方法样品以混合溶剂超声提取、Florisil固相萃取小柱净化处理后,采用DB-1701毛细管气相色谱柱分离样品,电子捕获检测器检测。内标法定量,计算有机氯农药的残留量。结果15种农药在5~500μg.L-1范围内具有良好的线性关系,相关系数均大于0.995。15种农药3个不同浓度的平均回收率为83.1%~110.6%,RSD%为3.4%~14.8%。最小检测量为0.08~1.5μg.L-1。被测样品中均含有不同程度的有机氯农药。结论本法简便、灵敏、准确、重现性好,可用于中药材中有机氯类农药的残留量测定。 相似文献
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固相萃取毛细管气相色谱法测定党参、龙胆中15种有机氯农药的残留量 总被引:5,自引:1,他引:5
目的用固相萃取毛细管气相色谱分析方法测定党参、龙胆2种中药材中15种有机氯农药残留量。方法样品以混合溶剂超声提取、Florisil固相萃取小柱净化处理后,采用DB 1701毛细管气相色谱柱分离样品,电子捕获检测器检测,内标法定量。结果15种农药在5~500μg.L-1内具有良好的线性关系,相关系数均大于0.995 0。15种农药3个不同质量浓度的平均回收率为83.1%~110.6%,RSD为3.4%~14.8%。最小检测量为0.08~1.50μg.L-1。被测样品中均含有不同程度的有机氯农药。结论本法可用于中草药党参和龙胆中有机氯类农药的残留量测定。 相似文献
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固相萃取技术在中药分析中的应用 总被引:1,自引:0,他引:1
目的 为复杂中成药有效成分分析和固相萃取技术的应用提供思路.方法 从7个方面总结了固相萃取技术在复杂中成药有效成分分析中的应用实例及实践经验.结果与结论 固相萃取技术可在复杂中药分析的前处理方面发挥越来越大的作用. 相似文献
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固相萃取-气相色谱串联质谱法测定温莪术中19种有机氯和有机磷农药残留 总被引:1,自引:0,他引:1
目的:建立固相萃取-气相色谱串联质谱法测定温莪术中11种有机磷和8种有机氯农药残留,对10种不同批次的温莪术样品进行农药残留测定。方法:温莪术样品用有机溶剂萃取法进行提取,提取溶剂选为乙腈,C18固相萃取小柱净化提取液,用气相色谱-质谱仪分析,采用选择离子模式测定,外标法定量。结果:19种农药成分的峰面积与其质量浓度均有良好的线性关系,相关系数在0.991~1.000。19种农药成分的加标回收率为60.5%~109.3%,RSD为3.9%~10.5%。结论:该方法简便、快速,灵敏度高,重复性好,能够准确地检测温莪术中19种农药残留。 相似文献
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萃取技术在生物样品中毒物的提取与富集中的应用 总被引:3,自引:0,他引:3
提取与富集是生物样品中毒物分析的关键步骤,本综述了各种萃取技术在此领域中的应用,分别论述了溶剂萃取,固相萃取,固相微萃取,超临界流体萃取和亲和萃取等技术的特点,局限性及应用实例,为应用及发展生物样品中毒物萃取技术提取了参考。 相似文献
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Phase transformation considerations during process development and manufacture of solid oral dosage forms 总被引:6,自引:0,他引:6
The quality and performance of a solid oral dosage form depends on the choice of the solid phase, the formulation design, and the manufacturing process. The potential for process-induced solid phase transformations must be evaluated during design and development of formulations and manufacturing processes. This article briefly reviews the basic principles of polymorphism, defines the classes of phase transformation and the underlying transformation mechanisms, and discusses respective kinetic factors. The potential phase transformations associated with common unit operations employed in manufacturing solid oral dosage forms are highlighted. Specific examples are given to illustrate the importance of solid phases, and process-induced phase transitions in formulation and process development. 相似文献
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Inès Gana Maria Barrio Bernard Do Josep-Lluís Tamarit René Céolin Ivo B. Rietveld 《International journal of pharmaceutics》2013
Understanding the phase behavior of an active pharmaceutical ingredient in a drug formulation is required to avoid the occurrence of sudden phase changes resulting in decrease of bioavailability in a marketed product. Benzocaine is known to possess three crystalline polymorphs, but their stability hierarchy has so far not been determined. A topological method and direct calorimetric measurements under pressure have been used to construct the topological pressure–temperature diagram of the phase relationships between the solid phases II and III, the liquid, and the vapor phase. In the process, the transition temperature between solid phases III and II and its enthalpy change have been determined. Solid phase II, which has the highest melting point, is the more stable phase under ambient conditions in this phase diagram. Surprisingly, solid phase I has not been observed during the study, even though the scarce literature data on its thermal behavior appear to indicate that it might be the most stable one of the three solid phases. 相似文献
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目的介绍近年来NMR技术在固相合成中的应用情况及进展。方法根据常见的用于测定核磁共振信号的原子核的不同 ,对核磁共振光谱进行分类叙述。结果与结论对于固相合成 ,传统的分析方法不适合分析与树脂相连的化合物 ,严重限制了固相合成的进一步发展。随着魔角自旋技术等一系列新技术的发展和应用 ,NMR光谱法不仅可以基本满足固相合成的需要 ,还能在一定程度上促进它的发展。 相似文献
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Choi YK Poudel BK Marasini N Yang KY Kim JW Kim JO Choi HG Yong CS 《International journal of pharmaceutics》2012,434(1-2):264-271
The objective of the present study was to enhance solubility and bioavailability of itraconazole by a combined use of membrane emulsification and spray drying solidification technique. A shirasu-porous-glass (SPG) membrane with a mean pore size of 2.5 μm was used to produce monodispersed microemulsions of itraconazole consisting of methylene chloride as the dispersed phase, a mixture of Transcutol HP and Span 20 as a stabilizer, and dextran as solid carrier dissolved in water as the continuous phase. The dispersed phase permeated through the SPG membrane into the continuous phase at an agitator speed of 150 rpm, a feed pressure of 15 kPa and a continuous phase temperature of 25°C and the resultant emulsion was solidified using spray-drying technique. Solid state characterizations of the solid emulsion showed that the crystal state of itraconazole in solid emulsion was converted from crystalline to amorphous form. The solid emulsion of itraconazole displayed a significant increase in the dissolution rate than that of pure itraconazole. Furthermore, the solid emulsion after oral administration gave about eight-fold higher AUC and about ten-fold higher C(max) in rats than pure itraconazole powder (p<0.05), indicating this formulation greatly improved the oral bioavailability of drug in rats. Thus, these results demonstrated that the SPG membrane emulsification system combined with spray-drying technique could be used as a promising technique to develop solid formulation of itraconazole with enhanced solubility and bioavailability. 相似文献
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Inhibition of a solid phase reaction among excipients that accelerates drug release from a solid dispersion with aging 总被引:2,自引:0,他引:2
Mizuno M Hirakura Y Yamane I Miyanishi H Yokota S Hattori M Kajiyama A 《International journal of pharmaceutics》2005,305(1-2):37-51
Hydrophobic drug substances can be formulated as a solid dispersion or solution using macromolecular matrices with high glass transition temperatures to attain satisfactory dissolution. However, very few marketed products have previously relied on solid dispersion technology due to physical and chemical instability problems, and processing difficulties. In the present study, a modified release product of a therapeutic drug for hypertension, Barnidipine hydrochloride, was developed. The drug product consisted of solid dispersion based on a matrix of carboxymethylethylcellulose (CMEC), which was produced using the spray-coating method. An enteric coat layer was sprayed on the surface of the solid dispersion to control drug release. Interestingly, the release rate accelerated as the drug product aged, while there were no indications of deceleration of the release rate which was due to crystallization of the drug substance. To prevent changes in the dissolution kinetics during storage periods, a variety of processing conditions were tried. It was found that not only use of non-aqueous solvents but also a reduction in coating temperatures consistently resulted in stable solid dispersions. The molecular bases of dissolution of the drug substance from those matrices were investigated. The molecular weight of CMEC was found to be a dominant factor that determined dissolution kinetics, which followed zero-order release, suggesting an involvement of an osmotic pumping mechanism. While dissolution was faster using a higher molecular weight CMEC, the molecular weight of CMEC in the drug product slowly increased with aging (solid phase reaction) depending on the processing conditions, causing the time-induced elevation of dissolution. While no crystalline components were found in the solid dispersion, the amorphous structure maintained a degree of non-equilibrium by nature. Plasticization by water in the coating solution relaxed the amorphous system and facilitated phase separation of the drug substance and CMEC upon production. The solid phase reaction advanced differentially in the solid dispersion depending on the degree of phase separation set initially. The use of non-aqueous solvents and/or a decrease in the coating temperatures inhibited the occurrence of phase separation upon production, thereby preventing the formation of CMEC-rich phases where the solid phase reaction occurred during storage. 相似文献
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Mills DA Fekrazad HM Verschraegen CF 《Current opinion in investigational drugs (London, England : 2000)》2008,9(6):647-657
Sunesis Pharmaceuticals Inc, under license from Dainippon Sumitomo Pharma Co Ltd, is developing SNS-595, a naphthyridine cell cycle inhibitor and apoptosis stimulator, for the potential treatment of a variety of solid and hematological malignancies. Phase I clinical trials had been completed in several solid tumor types and phase II clinical trials had been completed in patients with small-cell lung cancer and NSCLC. A phase II clinical trial in patients with platinum-resistant ovarian cancer and phase I/II and phase II clinical trials in patients with acute leukemias were ongoing at the time of publication. 相似文献