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11.
Yuanzhong Yang Reinhard I. BoysenJamil Chowdhury Asif AlamMilton T.W. Hearn 《Analytica chimica acta》2015
In this study, the advantages of carrying out the analysis of peptides and tryptic digests of proteins under gradient elution conditions at pH 6.5 by reversed-phase liquid chromatography (RP-HPLC) and in-line electrospray ionisation mass spectrometry (ESI-MS) are documented. For these RP separations, a double endcapped, bidentate anchored n-octadecyl wide pore silica adsorbent was employed in a capillary column format. Compared to the corresponding analysis of the same peptides and protein tryptic digests using low pH elution conditions for their RP-HPLC separation, this alternative approach provides improved selectivity and more efficient separation of these analytes, thus allowing a more sensitive identification of proteins at different abundance levels, i.e. more tryptic peptides from the same protein could be confidently identified, enabling higher sequence coverage of the protein to be obtained. This approach was further evaluated with very complex tryptic digests derived from a human plasma protein sample using an online two-dimensional (2D) strong cation-exchange (SCX)-RP-HPLC-ESI-MS/MS system. Again, at pH 6.5, with mobile phases of different compositions, improved chromatographic selectivities were obtained, concomitant with more sensitive on-line electrospray ionisation tandem mass spectrometric (ESI-MS/MS) analysis. As a consequence, more plasma proteins could be confidently identified, highlighting the potential of these RP-HPLC methods with elution at pH 6.5 to extend further the scope of proteomic investigations. 相似文献
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13.
Bipolar membrane electrodialysis is used in a three-compartment configuration to regenerate formic acid and sodium hydroxide from sodium formate. A previous study showed that the diffusion of molecular formic acid induces the loss of acid current efficiency. The present study shows the following results: the diffusion of molecular formic acid through the bipolar membrane explains quantitatively the presence of sodium formate in the sodium hydroxide solution. The loss of acid current efficiency is only due to diffusion of molecular acid through both anion-exchange and bipolar membranes. The sodium hydroxide current efficiency is determined by acid diffusion through the bipolar membrane and OH− leakage through the cation-exchange membrane. The flux of acid diffusion through the membranes is proportional to acid concentration and depends on sodium hydroxide concentration for bipolar membrane and on sodium formate concentration for anion-exchange membrane. The flux rates vary with temperature. 相似文献
14.
An on-line solid-phase extraction (SPE)-HPLC method was developed for simultaneous screening of nicardipine and amlodipine in human plasma. A short monolithic poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate) [p(GMA-EDMA)]-based weak cation-exchange (WCX) column was prepared and employed as the selective extraction sorbent, which exhibited good permeability and biocompatibility. During the on-line SPE protocol, high-abundance proteins (human serum albumin, immunoglobulin G, immunoglobulin A and transferrin) and most matrixes in plasma were fast removed while nicardipine and amlodipine were effectively trapped on this monolithic column. Furthermore, the monolithic WCX sorbent could be continuously reused more than 300 times without obvious changes in analytes extraction and proteins cleanup. The proposed method was linear over a range of 0.5-50.0 ng mL−1 for both analytes with a linear regression coefficient greater than 0.998, and the limit of detection (LOD) for each analyte was 0.2 ng mL−1. Validation assays also demonstrated acceptable precision and adequate recovery for simultaneous quantitative screening of nicardipine and amlodipine in human plasma. Real plasma samples from hypertensive patients receiving a dosing of 5 mg antagonists were examined by using the proposed method. Results indicated that the on-line SPE-HPLC method could be applied for simultaneously monitoring of nicardipine and amlodipine in clinical plasma samples. 相似文献
15.
建立了阳离子交换-电雾检测器测定CO2吸收液中一乙醇胺、二乙醇胺、N-甲基二乙醇胺的分析方法.实验采用IonPac CS17阳离子交换柱,选用甲酸与乙腈溶液为淋洗液,并考察了色谱柱种类、淋洗液种类与浓度对分离测定有机醇胺的影响.所测3种有机醇胺的检出限分别为0.21、0.04、0.32μg·mL-1,线性范围在1.0100μg·mL-1,相关系数分别为0.999 60、.999 3和0.999 2,加标回收率为87%98%.用所建立的方法测定了CO2吸收液中有机胺质量浓度,结果令人满意. 相似文献
16.
以乙烯基树脂为单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,偶氮二异丁腈(AIBN)为引发剂,十二醇为制孔剂,经原位聚合法制备了聚(乙烯基酯树脂-乙二醇二甲基丙烯酸酯)整体柱,然后在该柱上接入γ-缩水甘油基氧丙基三甲氧基硅烷,再用0.1 mol/L HCl和100 g/L NaHSO3处理后制成阳离子交换整体柱.考察了α-淀粉酶和溶菌酶在该柱上的分离,并对蛋清中的蛋白进行了分离.结果表明,等电点不同的蛋白在合适的pH条件下都能得到较好地分离. 相似文献
17.
新型强阳离子交换聚合物整体柱的制备及其在奶制品中三聚氰胺测定中的应用 总被引:1,自引:1,他引:0
在内径为530 μm的石英毛细管中原位聚合得到一种新的强阳离子交换聚合物整体柱2-丙烯酰胺-2-甲基-1-丙磺酸-乙二醇二甲基丙烯酸酯聚合物(poly(AMPS-co-EDMA))整体柱,并将其作为聚合物整体柱微萃取(PMME)的萃取介质。优化N,N-二甲基甲酰胺(DMF)和聚乙二醇(PEG)致孔体系的比例,制备得到的poly(AMPS-co-EDMA)整体柱渗透性好、机械强度高且在水溶液中具有良好的稳定性。通过考察样品溶液的pH值、盐浓度和有机溶剂含量对萃取效率的影响,证明该整体柱主要通过强阳离子交换和疏水相互作用对三聚氰胺进行萃取富集。在PMME与高效液相色谱联用技术的基础上,建立了检测奶制品中三聚氰胺含量的分析方法。奶制品中三聚氰胺的检出限和定量限分别为0.09 mg/kg和0.3 mg/kg,在0.5~80 mg/kg的含量范围内具有良好的线性关系,日内、日间测定的相对标准偏差不高于7.5%。结果表明,该方法简便、快速、灵敏度高且成本低,适合于奶制品中微量三聚氰胺的检测。 相似文献
18.
膨润土矿尚属本省缺门矿种。本文通过对贵州西部鸡场坪膨润土矿的物化性能测试,对所获得的实际资料进行分析研究,确定了该区矿石的属性及工业价值。经过野外对该区局部地段的地质评价,肯定了该矿的经济价值。鸡场坪嘭润土矿对地方经济的发展具有一定的实际意义。 相似文献
19.
许绍权 《华南师范大学学报(自然科学版)》1988,(2):1
本文应用阳离子交换法研究了在高氯酸的酸性介质中,于25℃下离子强度μ=4时,钪与Cl~-、Br~-和I~-的配位作用.测定的钪与卤离子配合物的稳定常数,氯离子体系为β_1=1.9和β_2=0.88;溴离子体系为β_1=0.58和β_2=0.44以及碘离子体系为β_1=0.43和β=0.12.较小的稳定常数值表明,钪与氯溴和碘离子不会形成稳定的π键配合物.其稳定常数呈现Cl~->Br~->I~-的递降顺序. 相似文献
20.
强酸性阳离子交换树脂催化合成甘油三乙酸酯的研究 总被引:2,自引:1,他引:1
王树清 《南通大学学报(自然科学版)》2005,4(1):25-27
以乙酸、甘油为原料,直接酯化合成甘油三乙酸酯,研究了反应温度、反应时间、原料配比、带水剂、催化剂用量等条件对合成反应的影响,确定了最佳工艺条件。该方法合成甘油三乙酸酯的最佳工艺条件是:反应温度92~98℃;反应时间5h;n(乙酸):n(甘油)为4.5:1.0;催化剂用量为总物料质量的0.9%;带水剂苯用量为15mL(甘油为0.15mol的情况下)。甘油三乙酸酯的收率达到92.30%。催化剂不经处理可循环使用多次。该催化剂具有价廉易得、催化活性好、不腐蚀设备、无环境污染等优点。 相似文献