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121.
122.
利用柱切换液相色谱,建立了参附注射液中苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、次乌头碱和乌头碱6种乌头碱类生物碱,以及Rg1、Re、Rf、Rb1、Rc、Ro、Rb2、Rb3、Rd 9种人参皂苷的分析方法。首先利用强阳离子交换的在线固相小柱选择性富集和净化样品中生物碱类成分,优化了色谱条件;并采用EC-C18柱作为人参皂苷的分析柱,通过优化实验条件,结合柱切换方式,去除了样品中辅料等大极性基质成分对色谱柱的污染,实现了生物碱分析和人参皂苷分析的自动切换。结果显示,样品中的生物碱和人参皂苷分离良好,线性相关系数(r2)均大于0.999,连续进样精密度的相对标准偏差(RSD) < 2.0%,重复性的RSD < 2.0%;其中6种生物碱的平均回收率为95.1%~98.6%,检出限为4.0~8.2 ng/mL;9种人参皂苷的平均回收率为91.7%~104%。所构建的基于柱切换液相色谱技术的在线固相萃取方法能够有效去除样品中的基质干扰,快速完成参附注射液中3种单酯型生物碱和9种人参皂苷的快速定量,同时也可对3种双酯型生物碱进行限量检测,可应用于药物的质量评价。 相似文献
123.
毛细管气相色谱法分析虾蛄肉中的脂肪酸 总被引:2,自引:0,他引:2
以快速脂肪提取器分别提取雄、雌虾蛄肉中脂肪,利用50m×0.35mmi.d.PEG-20M玻璃毛细管柱分离测定了雄、雌虾蛄肉中的脂肪酸,结合气相色谱/质谱法,鉴定出45个峰,分别占脂肪酸总量的99.2%和98.0%,其中不饱和脂肪酸分别为74.7%和71.5%。 相似文献
124.
Thomas H. Walter Bonnie A. Alden Kenneth Berthelette Jessica A. Field Nicole L. Lawrence Justin McLaughlin Amit V. Patel 《Journal of separation science》2022,45(8):1389-1399
We have characterized a sulfobetaine stationary phase based on 1.7 μm ethylene-bridged hybrid organic–inorganic particles, which is intended for use in hydrophilic interaction chromatography. The efficiency of a column packed with this material was determined as a function of flow rate, demonstrating a minimum reduced plate height of 2.4. The batch-to-batch reproducibility was assessed using the separation of a mixture of acids, bases, and neutrals. We compared the retention and selectivity of the hybrid sulfobetaine stationary phase to that of several benchmark materials. The hybrid sulfobetaine material gave strong retention for polar neutrals and high selectivity for methyl groups, hydroxy groups, and configurational isomers. Large differences in cation and anion retention were observed among the columns. We characterized the acid and base stability of the hybrid sulfobetaine stationary phase, using accelerated tests at pH 1.3 and 11.0, both at 70°C. The results support a recommended pH range of 2–10. We also investigated the performance of columns packed with this material for metal-sensitive analytes, comparing conventional stainless steel column hardware to hardware that incorporates hybrid surface technology to mitigate interactions with metal surfaces. Compared to the conventional columns, the hybrid surface technology columns showed a greatly improved peak shape. 相似文献
125.
依据柱相比的热力学定义和反相液相色谱中溶质的计量置换保留理论(the stoichiometric dispheement heory of solute for retention,SDT-R),对反相液相色谱中固定相和流动相性质、温度对柱相比的影响进行了研究。结果表明:固定相的种类和配基的疏水性对柱相比影响较大,而流动相中有机溶剂的种类,特别是脂肪酸作为置换剂时,对柱相比的影响更大,而柱相比受温度的影响较小。此外,通过用27种小分子溶质对柱相比的测定,其logI和Z良好的线性关系,进一步证明柱相比是一个与溶质性质无关的常数。 相似文献
126.
127.
Changming Cheng Tao Jiang Jun Han Kai Lv Sheng Hu Xiaolin Wang 《Electrophoresis》2016,37(20):2657-2662
In this study, in‐column fiber‐optic (ICFO) laser‐induced fluorescence (LIF) detection technique is coupled with capillary electrophoresis (CE) for the rapid separation of neodymium for the first time. The effects of buffer concentration, buffer pH, and separation voltage on the CE behaviors, including electrophoretic efficiency and detection sensitivity, are investigated in detail. Under the optimal condition determined in this study (15 mM borate buffer, pH 10.50, separation voltage 24 kV), neodymium could be separated effectively from the neighboring lanthanides (praseodymium and samarium) within several minutes, and the limit of detection for neodymium is estimated to be at the ppt level. The ICFO‐LIF‐CE system assembled in this study exhibits unique performance characteristics such as low cost and flexibility. Meanwhile, the separation efficiency and detection sensitivity of the assembled CE system are comparable to or somewhat better than those obtained in the previous traditional CE systems, indicating the potential of the assembled CE system for practical applications in the fields of spent nuclear fuel analysis, nuclear waste disposal/treatment, and nuclear forensics. 相似文献
128.
In this second part of the series of investigations involving the postpolymerization modification of a hydroxy monolith (OHM) capillary column, the surface hydroxyl groups were reacted with epoxy biphenyl thus yielding the so‐called Biphenyl OHM capillary column. The modification involved the epoxy ring opening of the 2‐biphenylyl glycidyl ether catalyzed by BF3 and its subsequent reaction with the hydroxyl groups on the OHM precursor surface. The Biphenyl OHM capillary column thus obtained exhibited the typical reversed phase behavior by primarily hydrophobic interactions vis‐à‐vis the homologous series of alkyl benzenes and in addition by π–π interactions toward nitroalkane homologous series via their π‐electron rich nitro groups. This dual retention mechanism was very distinctly observed with a set of PAH solutes in the sense that the k values of the PAH solutes were comparable to those obtained on a more non polar stationary phase, namely the Epoxy OHM C‐16 reported in the preceding article. Other aromatic solutes showed the dual retention mechanism on the Biphenyl OHM capillary including phenols, anilines derivatives, and phenoxy acid herbicides. The Biphenyl OHM capillary exhibited good reproducibility from run‐to‐run, day‐to‐day, and column‐to‐column. 相似文献
129.
Electrospray ionization mass spectrometric detection of low polar compounds by adding NaAuCl4 下载免费PDF全文
Hiroshi Moriwaki 《Journal of mass spectrometry : JMS》2016,51(11):1096-1102
Liquid chromatography electrospray ionization mass spectrometry (LC/ESI/MS) has been widely used for various analyses. However, it is difficult to use LC/ESI/MS for the analysis of low polar compounds, such as polycyclic aromatic hydrocarbons. It is well known that AuCl4? ion decomposes to AuCl3 by heating, and AuCl3 is a strong π‐electrophilic Lewis acid. Low polar compounds (pyrene, benzo[a]pyrene, perylene, benzo[ghi]perylene, dibenzothiophene and p‐dimethoxybenzene) were detected by ESI/MS in the positive ion mode by adding NaAuCl4. The low polar compound interacts with AuCl3 formed at the ESI interface, and undergoes electron transfer to AuCl3. The radical cation of the low polar compound was then detected by MS. In addition, the LC/ESI/MS determination of polycyclic aromatic hydrocarbons by the post‐column addition of NaAuCl4 was studied. © 2016 The Authors Journal of Mass Spectrometry Published by John Wiley & Sons Ltd 相似文献
130.