316 resultados para HPLC-APCI-MS
Resumo:
本文采用 5 5MeV u1 2 C6+离子注入鬼臼衍生物之一———鬼臼乙叉甙 (VP1 6) ,针对它在临床上的缺点 ,试图利用重离子的能量转移和质量沉积对其分子组成与结构进行改造 ,以增加它的水溶性 ,提高疗效 ,减小毒性。实验样品在离子注入后 ,先后进行了紫外 (UV)、高效液相 (HPLC)和液质联用 (HPLC -MS)分析 ,并对癌细胞K5 6 2和HL- 6 0分别进行了药理活性测定 ,取得了初步结果和进行了简短讨论。
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这篇论文里,我们对基于ms Windows的微机γ谱分析程序的数学原理,算法及程序设计进行了阐述;同时,我们也介绍了测试结果,此结果表明了拟合过程的高效性,高稳定性与准确性,并且,程序计算出的峰面积也是可接受的。 在第一部分里,全面阐述了数学原理与算法,包括由M. A. Mariscotti设计且已衍生出许多新算法的叫作DIFDIF的找峰算法,由BFGS方法实现的以χ2为拟合优值的拟合过程,在求峰下净面积及进行系统刻度中需要使用的公式等等。这些内客构成了γ谱分析程序设计哲学的核心,也是本论文的重点。 第二章里,我们一方面概括地介绍了基于面向对象思想的从系统分析到设计整个过程的系统开发文档;另一方面,我们也介绍了一些有用的程序片段,它们或者关于C++或MS Windows程序设计方法,或者关于运行时间错的处理。
Resumo:
建立了气相色谱-质谱-选择离子监测(GC-MS-SIM)同时测定土壤中10种农药(三嗪类除草剂、酰胺类除草剂和有机氯农药)的多残留分析方法.样品采用正己烷/丙酮(1:1,V/V)超声提取、氟罗里硅土柱层析净化、GC-MS-SIM测定.10种农药在0.01(0.02)—1.0(2.0)mg.l-1范围内线性良好,相关系数介于0.9963—0.9998之间;在10,50和250ng.g-1添加水平下,平均回收率介于81%—117%之间,相对标准偏差均小于14.4%;方法检出限达到ppb至sub-ppb级(0.1—1.3ng.g-1).将此方法应用于辽宁省不同性质土壤中70个实际土壤样品的分析,阿特拉津、乙草胺、六氯苯、丁草胺、狄氏剂和艾氏剂有检出,该法对不同性质土壤具有广泛适用性.
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Reversed-phase high performance liquid chromatography (RP-HPLC) was employed to develop predictive models for fish bioconcentration factors (BCF) of organic compounds. Estimation of BCF from RP-HPLC retention parameters on octadecyl-bonded silica gel (ODS), cyanopropyl-bonded silica gel (CN), and phenyl-bonded silica gel (Ph) columns were investigated. The results show that, for a set of compounds belonging to different chemical classes, the CN stationary phase is the best one among the three columns and better than n-octanol/water model for BCF estimation. A multi-column RP-HPLC model, using the retention parameters on the CN and Ph columns as the variables of multiple linear regression equations, was further evaluated to estimate BCF of organic compounds belonging to different chemical classes, and the results show that the multi-column RP-HPLC model is better than that of any single RP-HPLC column for BCF estimation.
Resumo:
Since protein phosphorylation is a dominant mechanism of information transfer in cells, there is a great need for methods capable of accurately elucidating sites of phosphorylation. In recent years mass spectrometry has become an increasingly viable alternative to more traditional methods of phosphorylation analysis. The present study used immobilized metal affinity chromatography (IMAC coupled with a linear ion trap mass spectrometer to analyze phosphorylated proteins in mouse liver. A total of 26 peptide sequences defining 26 sites of phosphorylation were determined. Although this number of identified phosphoproteins is not large, the approach is still of interest because a series of conservative criteria were adopted in data analysis. We note that, although the binding of non-phosphorylated peptides to the IMAC column was apparent, the improvements in high-speed scanning and quality of MS/MS spectra provided by the linear ion trap contributed to the phosphoprotein identification. Further analysis demonstrated that MS/MS/MS analysis was necessary to exclude the false-positive matches resulting from the MS/MS experiments, especially for multiphosphorylated peptides. The use of the linear ion trap considerably enabled exploitation of nanoflow-HPLC/MS/MS, and in addition MS/MS/MS has great potential in phosphoproteome research of relatively complex samples. Copyright (C) 2004 John Wiley Sons, Ltd.