期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1218, 期 46, 页码 8411-8422出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2011.09.057
关键词
Multivariate curve resolution; Alternating least squares; LC x LC; Comprehensive two dimensional liquid chromatography; Phase shifts; Rank deficiencies
资金
- National Science Foundation [CHE-0911330]
- Direct For Mathematical & Physical Scien
- Division Of Chemistry [0911330] Funding Source: National Science Foundation
- Direct For Mathematical & Physical Scien
- Division Of Chemistry [0911516] Funding Source: National Science Foundation
There has been a tremendous increase in research on comprehensive two dimensional LC (LC x LC); however, to date, the central analytical issue, quantification, has received only minimal attention. It is vital to the further development of LC x LC that a greater understanding of the specific factors affecting peak quantification in LC x LC be attained. This work focuses on the following factors: data complexity, retention time shifting, dynamic range issues, chromatographic and spectral peak overlap and difficulties related to background signal removal. The above mentioned factors that affect peak quantification are investigated using fourteen replicate analyses of a urine sample, representing the effects of such factors when analyzing samples in complex matrices. We demonstrate that quantification of LC x LC data is improved following implementation of chemometric techniques that minimized the deleterious effects on quantification due to chromatographically overlapped peaks, retention time shifting and background signal interference. The chemometrically resolved data shows a 2.5-fold increase in precision of quantification over the quantification of the raw data. It is also demonstrated that the method quantifies sixteen peaks that were not visually evident prior to chemometric analysis. The purpose of this paper is to determine the impact of these issues on the effectiveness of LC x LC as a technique for the quantitative analysis of complex samples. (C) 2011 Elsevier B.V. All rights reserved.
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