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题名: Pressurized capillary electrochromatographic assay of trimethoprim impurities using 1 mu m particle-based columns
作者: Qu, Qi Shu;  Mangelings, Debby;  Shen, Fei;  Hu, Xiao Ya;  Yan, Chao;  Zhang, Yu Kui;  Heyden, Yvan Vander
关键词: capillary columns ;  micronsized particles ;  pressurized capillary electrochromatography ;  trimethoprim
刊名: JOURNAL OF CHROMATOGRAPHY A
发表日期: 2007-10-26
DOI: 10.1016/j.chroma.2007.08.068
卷: 1169, 期:1-2, 页:228-234
收录类别: SCI
文章类型: Article
WOS标题词: Science & Technology ;  Life Sciences & Biomedicine ;  Physical Sciences
类目[WOS]: Biochemical Research Methods ;  Chemistry, Analytical
研究领域[WOS]: Biochemistry & Molecular Biology ;  Chemistry
英文摘要: One micrometre silica particles, derivatized with C18, were electrokinetically packed into a 75-mu m-i.d. capillary. The resulting column was evaluated for the separation of trimethoprim (TMP) and its impurities using pressurized capillary electrochromatography (pCEC), starting from a capillary liquid chromatographic (CLC) separation. These samples require gradient elution when separated by high performance liquid chromatography (HPLC), but with the new columns isocratic elution suffices for their separation by CLC or pCEC. Only 70,000 theoretical plates/m for impurity C were achieved using CLC mode at relative low pressure (78 bar) although very small particles were utilized. When a voltage above 2 W (50 V/cm) was applied, unknown peaks appeared, which was assumed due to an electrophoretic effect with the unknown peaks resolving as a result of the applied voltage. In order to minimize these unfavorable contributions, only a low voltage was applied, still leading to higher separation performances and shorter separation times than in CLC. The optimal analyzing conditions in pCEC included a pressure of 78 bar, an applied voltage of I W, and a mobile phase consisting of 80 mM sodium perchlorate (pH 3.1)/methanol (60/40, v/v). These conditions were used to separate and quantify four major impurities in TMP within 22 min. The obtained calibration curves were linear (r > 0.9980) in concentration ranges between 0.005 and 0.1 mg/mL for impurities A and C; 0.02 and 0.10 mg/mL for impurity F; and 0.01 and 0.10 mg/mL for impurity H. The detection limits (S/N = 3) for impurities A, C, F, and H were 0.52, 0.84, 3.18, and 2.41 mu g/mL, respectively. The calibration curves were successfully applied to analyze spiked bulk samples, with mean recoveries ranging from 92% to 110%. The developed method can therefore be considered simple, rapid, and repeatable. (c) 2007 Elsevier B.V. All rights reserved.
关键词[WOS]: CHROMATOGRAPHY-MASS-SPECTROMETRY ;  LIQUID-CHROMATOGRAPHY ;  ELECTRIC-FIELD ;  SEPARATION ;  PEPTIDES
语种: 英语
WOS记录号: WOS:000250316400023
Citation statistics: 
内容类型: 期刊论文
URI标识: http://cas-ir.dicp.ac.cn/handle/321008/140700
Appears in Collections:中国科学院大连化学物理研究所_期刊论文

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作者单位: 1.Vrije Univ Brussels, Dept Analyt Chem & Pharmaceut Technol, B-1090 Brussels, Belgium
2.Yangzhou Univ, Coll Chem & Chem Engn, Jiandsu Key Lab Environm Mat & Environm Engn, Yangzhou 225002, Peoples R China
3.Chinese Acad Sci, Dalian Inst Chem Phys, Natl Chromatog R&A Ctr, Dalian 116011, Peoples R China
4.Shanghai Jiao Tong Univ, Sch Pharm, Shanghai 200030, Peoples R China

Recommended Citation:
Qu, Qi Shu,Mangelings, Debby,Shen, Fei,et al. Pressurized capillary electrochromatographic assay of trimethoprim impurities using 1 mu m particle-based columns[J]. JOURNAL OF CHROMATOGRAPHY A,2007,1169(1-2):228-234.
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