摘要
化学计量学是化学的重要的分支学科,可被认为是一门运用数学、统计学、计算机科学以及其它相关学科的理论与方法,结合现代仪器分析技术,以“数学分离”部分或完全替代“化学分离”,被广泛用于复杂体系中的目标物的定性定量分析的学科。其独特的分离理论及特性,正越来越引起化学家们的关注。色谱技术是当前最普通使用的检测技术,在分离复杂体系,对多组分的同时测定方面发挥了重要的作用。本文对化学计量学中的多维校正方法结合色谱技术的理论及应用方面进行了一些探索研究,取得系列创新性成果,其主要内容包括以下几方面:
1.二阶校正方法结合HPLC-DAD用于复杂药物体系定量分析(第二章-第五章)
对药物进行准确、快速定量分析是现代生命科学领域中一项重要的内容,对监控药品质量起着至关重要的作用。面对研究体系的日益复杂化和仪器产生数据的多维化,使用和研究适合的能在有大量未知干扰共存下,直接、快速和准确对样品中的感兴趣组分进行定性定量分析的方法,是所有分析化学学家们所密切关注的问题。当两种物质的分子结构式相似,化学性质也相近,或者体系中存在其它未知组分的干扰时,有时用简单的色谱条件很难将它们完全分离。因此,我们借助化学计量学二阶校正方法,并将其与HPLC-DAD结合用于对血浆中的甲硝唑和替硝唑以及美托洛尔和阿替洛尔药物的同时定量分析,获得了满意的结果,充分利用了二阶校正方法的“二阶优势”。
药物中同分异构体和对映体的分离也是分析化学家们很关注的问题。同分异构体具有相同的分子量,而且很多还具有相似的化学性质,这给实际的色谱分离带来了很大的因难。由于药物组成复杂,在色谱分析中,药物中的同分异构体之间以及与干扰物之间的色谱和光谱往往会存在部分或严重重叠,这给定量分析带来了困难,此时多采用比较复杂的色谱条件或用昂贵的专用色谱柱。本文利用二阶校正方法结合HPLC-DAD对实际药物样品体系中的同分异构体补骨脂素和异补骨脂素以及土木香内脂和异土木香内脂进行了分析研究,在仅经过简单的样品预处理后,无需复杂的色谱条件,借助化学计量学的“数学分离”部分或完全替代“化学分离”,获得了满意的结果。为了验证方法的可靠,还分别用LC/MS和GC/MS进行了验证实验,结果无显著性差异。化学计量学相对于传统的色谱方法的优势在于,在色谱峰有部分甚至严重重叠的情况下仍能对感兴趣组进行定性或定量分析,这也正是二阶校正方法的“二阶优势”的体现。为复杂药物样品中成分的定量分析提供了一种新的分析方法。
2.三线性二阶校正方法用于HPLC-DAD重叠色谱分析(第六章)
在应用的基础上,本文还对三线性二阶校正方法解析色谱重叠方面进行了研究。以归一化之后的分离度或重叠度来表示重叠组分的色谱或光谱的重叠程度,此法最大优点就是使重叠峰尤其是包埋峰中各组分的差异性更加明显化。对模拟数据和实际检测数据进行了分析,结果表明只要是重叠组分归一化之后的色谱和光谱不完全重叠并且色谱和光谱的重叠不同时极大到一定程度时,即使是大色谱峰包小色谱峰的情况,三线性分解算法方法仍然能给出重叠各组分的分辨色谱和光谱,并能对其进行准确的定性定量分析。当色谱和光谱的重叠度越高,共线性越严重,分辨的峰形越嘈杂,在相同条件下,相对来说,重叠度越小,算法解析结果将会越好。
3.三阶校正结合二维HPLC-DAD用于复杂药物体系的定量分析(第七章)
随着分析仪器的发展和分析方法不断改进,大量高维数据的获得将变得越来越容易,三维二阶校正方法越来越满足不了需要,因此迫切需要能处理更高维数据的高维校正方法。目前,用于处理复杂四维数据的四线性三阶校正方法尚不多见。本文提出了四线性三阶校正方法交替四线性分解(AQLD)并同交替惩罚四线性分解(APQLD)以及四维平行因子分析(Four-way PARAFAC)算法,对LC×LC-DAD检测川芎样品中阿魏酸得到的四维数据进行了四线性分解分析,获得了比较准确的结果。同时对这三种算法解析实际数据的特点进行了比较。结果表明,三阶校正非常适合解析LC×LC-DAD产生的四维数据阵,三阶校正方法能利用色谱峰重叠组分间的差异信息(色谱保留值和光谱的不同)对感兴趣组分的色谱和光谱进行准确的分辨。在模拟和真实测定体系中,总体上新算法AQLD和APQLD算法的性能要稍优于Four-way PARAFAC算法。相对二阶校正方法,三阶校正方法目前还处于起步发展阶段,其复杂的“三阶优势”或更高阶优势还需要不断探索。
Chemometrics is a developing composite discipline, which is an important branch of the analytical chemistry and widely used to the qualitative and quantitative analysis for the analytes in complex system. Its unique characteristics, "mathematical separation" partially or completely replace "chemical separation", which is increasingly causing the concern of chemists. Now chromatographic techniques play an important role in simultaneous determination of multiple components in samples. In this paper, the research work focuses on multi-way calibration combined with chromatographic techniques for quantitative analysis of interest in complex chemical systems.
1. Second-order calibration coupled with HPLC-DAD for quantitative analysis of drugs in complex systems (Chapter 2 to Chapter 5)
Accurate, rapid and quantitative determination of ingredient is an important thing in life science and plays an important role in drug quality control. Quantitative analysis of components of interesting even in the presence of unknown interferences is the most concern of analysts. Two components are difficult to be separated by simple chromatographic condition as they have similar structure and characteristic, accordingly, methods of chemometrics are used to helpfully resolve this problem. Second-order calibration methods were presented to allow accurate and reliable quantitative analysis of metronidazole and tindazole, metoprotol and atenolol in plasma samples, which fully reflects the“second-order advantage”.
Isomeric compounds have the same molecular weight and many also have similar chemical properties, so it is unnecessary to surprise that they have similar spectral profiles and close retention times in chromatographic analysis. How to effectively separate and quantitatively analyze them in drugs is also the interesting question of analysts. Recently there are many papers to aim at these problems, but most methods often suffer from being time-consuming and needing tedious pretreatments in chromatography or too expensive cost. This study described that HPLC-DAD coupled with second-order calibration methods was employed to determine isomeric compounds such as psoralen and isopsoralen, alantolactone and isoalantolactone in Chinese tradional medicine. With the second-order calibration method, one can simplify the sample preparation procedure only by using a simple and convenient solvent extraction with methanol. Thought isomeric compounds have not only similar spectral profiles and close retention times in chromatographic analysis, but also their profiles overlapping with those of unknown interference from complex system. Nevertheless second-order calibration methods could provide accurate concentration prediction and good resolution of elution and spectral profiles for the analytes of interests under this circumstance. Also LC/MS and GC/MS were performed to validate the accuracy of results which were obtained by second-order calibration methods. The results showed that second-order calibration methods is a powerful chemometric tool to decompose heavily overlapped peaks into their pure chromatographic, spectral and concentration profiles even in complicated systems such as pharmaceutical preparations. The second-order advantage was fully exploited in this paper, which made concentration prediction feasible even in the presence of unknown interferences. In the present work, a simple sample disposal and short analysis time has been achieved. It has been proved that“mathematical separation”instead of partial“physical or chemical separation”was useful in chromatographic analysis. It provides a new method of quantitative analysis for ingredient in complex drug samples.
2. Quantitative analysis of overlapping chromatographic peaks using trilinear second-order methods (Chapter 6)
Base on the application in practice of trilinear second-order calibration methods, resolution of overlapping chromatograms using these decomposition algorithms are also detailly studied in this paper. Chromatographic and spectral peaks were normalized to calculate resolution or overlapping degree of components in overlapping peaks, which made the difference of components more obvious in overlapping peaks especially in embedded peaks. The results obtained by simulated and real data have shown that trilinear decomposition algorithms have the superior performance to resolve overlapping peaks of elution and spectral profiles and quantify the analytes as there is discrepancy among overlapping peaks or embedded peaks and overlap degree of chromatographic and spectra peaks are not simultaneous severely approximate 100%. With the same noise level and collinearity, the greater of separation of chromatographic and spectral peaks the better results are attained from the algorithms.
3. Third-order calibration coupled with LC×LC-DAD for quantitative analysis of drugs in complex systems (Chapter 7)
With the development of analytical instruments and methods, it becomes increasing easier to obtain a large number of high-dimensional data such as four-dimensional data which involve more information than second-dimensional data. It requires more effective higher-order calibration methods of chemometrics to derive useful information from it, accordingly, third-order calibration methods that came into being developed. In this paper, LC×LC-DAD coupled with AQLD (alternating quadrilinear decomposition), APQLD (alternating penalty quadrilinear decomposition) and four-way PARAFAC (parallel factor analysis) was applied to quantitatively determine ferulic acid in chuanxiong samples, acceptable results can be supplied. It come to a conclusion, three third-order calibration methods are adapted to analyze four-way data attained from two-dimensional HPLC-DAD. Comparing with AQLD, APQLD and four-way PARAFAC algorithms, obviously, AQLD and APQLD are generally insensitive to the overestimates of the component number chosen and have fast convergence rate, which is difficult for four-way PARAFAC to surpass. The accuracy of AQLD and APQLD is better than that of four-way PARAFAC illustrated by the EJCR test. The performances of both AQLD and APQLD were slightly better than that of four-way PARAFAC for decomposing quadrilinear data in this paper. Since an additional temporal dimension was introduced and more information of samples was considered, theoretically, third-order calibration could give a higher sensitivity and selectivity than second-order calibration, which can be considered as“third-order advantage”. Admittedly, the advantage of four-dimensional data analysis is still at an early stage of exploration, and complex or higher order advantage is still to be found and studied for us.
引文
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