化学计量学二阶校正法在荧光和色谱分析中的应用
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摘要
化学计量学是一门新兴发展的交叉学科,它运用数学、统计学、计算机科学等方法设计优化化学量测过程,并通过解析化学量测数据最大限度地获取化学及相关信息。
化学计量学二阶校正方法由于其具有“二阶优势”(Second-order advantage),可以解决一些传统方法无法处理的问题。将化学计量学二阶校正法与现代分析仪器相结合,以“数学分离”增强甚至代替“化学分离”时,可实现未知干扰共存下对一个乃至多个组分进行直接同时快速的定量测定。
本文作者通过利用三维荧光光谱及HPLC-DAD等现代分析仪器量测手段,结合化学计量学二阶校正法,在复杂多组分体系的定量分析方面进行了探索性应用基础研究。主要涉及以下几个方面:
在论文的第2章,利用激发-发射矩阵荧光光谱与化学计量学二阶校正方法相结合,实现了快速测定人体血浆样和牛蒡子中的牛蒡苷含量。采用二阶校正法中的平行因子分析(PARAFAC)和交替归一加权残差(ANWE)两种算法进行解析,实现了对血浆样中牛蒡苷含量的直接快速定量测定。此外,采用上述方法对牛蒡子中的牛蒡苷含量进行了快速测定,所得结果与液相色谱方法所得结果进行比较,结果令人满意。
大黄是一种传统中药材,其主要活性成分为蒽醌衍生物,其中包括有大黄素和大黄酚。本论文的第3章,尝试利用三维激发发射荧光光谱结合两种二阶校正方法,分别基于交替惩罚三线性分解(APTLD)算法和交替归一加权残差(ANWE)算法,对尿液样中背景干扰共存下的大黄素和大黄酚进行同时定量测定。尽管大黄素和大黄酚的荧光光谱重叠十分严重,且尿液样品中基体干扰目标物的分析,但采用这两种二阶校正方法解析这些三维荧光数据,仍能得到良好的分辨结果。遗憾的是由于尿液基质同大黄素之间可能发生了化学反应,引起大黄素荧光的淬灭,从而影响了大黄素的定量结果,因此,本章利用化学计量学二阶校正法与三维荧光相结合只能对尿液中大黄酚的含量进行准确定量测定。
美托洛尔和阿替洛尔均为第二代β1受体阻滞剂,临床上用于治疗高血压、冠心病、心律失常、甲亢等各种疾病。论文的第4章提出了采用反相高效液相色谱与化学计量学二阶校正方法相结合,对血浆和尿液中的美托洛尔和阿替洛尔进行同时测定。尽管美托洛尔和阿替洛尔的色谱和光谱峰均重叠严重,且样品中的基质干扰目标物的分析,但本章采用交替三线性分解(ATLD)算法解析色谱数据,利用“数学分离”增强“化学分离”,实现了未知干扰组分存在下,感兴趣组分美托洛尔和阿替洛尔的同时定量分析。
磺胺类(SAs)药物在奶牛业中的应用非常普遍。由于SAs在体内作用和代谢的时间较长,在动物源性食品中容易残留,危及人体健康。在论文的第5章,采用HPLC-DAD检测与交替惩罚三线性分解(APTLD)算法相结合对牛奶中的磺胺类兽药残留量进行了分析测定。尽管样品中组分分离不完全,并且存在大量干扰组分,但利用化学计量学二阶校正方法的“二阶优势”,仍能对该体系中感兴趣的磺胺组分给出准确的定量分析结果。
Chemometrics is a developing composite discipline of chemistry. The main focus of chemometrics is on applying the methods of mathematics, statistics and computer sciences to extracting chemical information, to designing the optimal scheme for chemical measurements and to elucidating the data collected from chemical measurements.
The second-order calibration methodologies can deal with some traditional difficult problems because of the second-order advantage. The chemometric methodologies coupled with higher-order analytical instruments can improve or replace the“chemical separation”with“mathematical separation”, enable accurate and reliable determination of the analyte concentrations even in the presence of uncalibrated interferents.
In this paper, the authors utilized the analytical instruments such as EEMs and HPLC-DAD, coupled with second-order calibration methodologies, and did some work in the research of complex multi-component systems. Studies presented in the thesis primarily deals with the following aspects:
In Chapter 2, it proposed a new approach for direct determination of arctiin content in plasma samples as well as a Chinese medicine (Arctium lappa L.) by the combination of excitation-emission matrix fluorescence and second-order calibration methods based on the parallel factor analysis (PARAFAC) and the alternating normalization-weighted error (ANWE) algorithms. The estimated content of arctiin in arctium lappa L. obtained by fluorescence determination was also satisfactory compared with that of the HPLC method. It can be seen that the suggested methods can be employed to directly determine arctiin, even in the presence of unknown and un-calibrated interferences, only with a simple pretreatment procedure.
The rhubarb is one of the most popular traditional Chinese herbal medicines. The main active constituents of rhubarb have been reported to be anthraquinones, such as emodin and chrysophanol. In Chapter 3, it was tried to use three-way excitation-emission matrix fluorescence combining chemometrics second-order calibration algorithms, including the alternating penalty trilinear decomposition (APTLD) algorithm and the alternating normalizationweigh (ANWE) algorithm, to determined emodin and chrysophanol even in presence of urine background interferents. Though the peaks of the analytes were heavily overlapped and urine background interferents coeluted with the compounds studied, good resolved results could be obtained. But it is a pity that the estimated content of the emodin is not acceptable, it maybe owe to the reaction of the emodin with the urin background interferents and then the fluorescence of emodin had been decreased. Thus, it only can obtained satisfactory estimated results of the chrysophanol in the urine by using the method mentioned.
In Chapter 4, HPLC-DAD coupled with chemometric second-order calibration method based on ATLD algorithm was applied toβ-adrenergic receptor-blocking agent in body fluids. Though the chromatographic and spectral peaks of the analytes were heavily overlapped and interferents coeluted with the compounds studied, good recoveries of the analytes could be obtained.
Sulfonamides constitute a group of drugs which are widely used in veterinary. Their metabolism process are slow in animal body, thus, residues of these drugs may remain in food of animal origin. In Chapter 5, a new method based on the use of HPLC-DAD coupled with the alternating penalty trilinear decomposition (APTLD) algorithm was applied to the rapid determination of sulfonamides in milk samples. Though the chromatographic and spectral peaks of the components were highly overlapped, good quantitative results could be obtained owing to the second order advantage. The application of second-order calibration methodologies provides a new technique to food analysis.
化学计量学二阶校正方法由于其具有“二阶优势”(Second-order advantage),可以解决一些传统方法无法处理的问题。将化学计量学二阶校正法与现代分析仪器相结合,以“数学分离”增强甚至代替“化学分离”时,可实现未知干扰共存下对一个乃至多个组分进行直接同时快速的定量测定。
本文作者通过利用三维荧光光谱及HPLC-DAD等现代分析仪器量测手段,结合化学计量学二阶校正法,在复杂多组分体系的定量分析方面进行了探索性应用基础研究。主要涉及以下几个方面:
在论文的第2章,利用激发-发射矩阵荧光光谱与化学计量学二阶校正方法相结合,实现了快速测定人体血浆样和牛蒡子中的牛蒡苷含量。采用二阶校正法中的平行因子分析(PARAFAC)和交替归一加权残差(ANWE)两种算法进行解析,实现了对血浆样中牛蒡苷含量的直接快速定量测定。此外,采用上述方法对牛蒡子中的牛蒡苷含量进行了快速测定,所得结果与液相色谱方法所得结果进行比较,结果令人满意。
大黄是一种传统中药材,其主要活性成分为蒽醌衍生物,其中包括有大黄素和大黄酚。本论文的第3章,尝试利用三维激发发射荧光光谱结合两种二阶校正方法,分别基于交替惩罚三线性分解(APTLD)算法和交替归一加权残差(ANWE)算法,对尿液样中背景干扰共存下的大黄素和大黄酚进行同时定量测定。尽管大黄素和大黄酚的荧光光谱重叠十分严重,且尿液样品中基体干扰目标物的分析,但采用这两种二阶校正方法解析这些三维荧光数据,仍能得到良好的分辨结果。遗憾的是由于尿液基质同大黄素之间可能发生了化学反应,引起大黄素荧光的淬灭,从而影响了大黄素的定量结果,因此,本章利用化学计量学二阶校正法与三维荧光相结合只能对尿液中大黄酚的含量进行准确定量测定。
美托洛尔和阿替洛尔均为第二代β1受体阻滞剂,临床上用于治疗高血压、冠心病、心律失常、甲亢等各种疾病。论文的第4章提出了采用反相高效液相色谱与化学计量学二阶校正方法相结合,对血浆和尿液中的美托洛尔和阿替洛尔进行同时测定。尽管美托洛尔和阿替洛尔的色谱和光谱峰均重叠严重,且样品中的基质干扰目标物的分析,但本章采用交替三线性分解(ATLD)算法解析色谱数据,利用“数学分离”增强“化学分离”,实现了未知干扰组分存在下,感兴趣组分美托洛尔和阿替洛尔的同时定量分析。
磺胺类(SAs)药物在奶牛业中的应用非常普遍。由于SAs在体内作用和代谢的时间较长,在动物源性食品中容易残留,危及人体健康。在论文的第5章,采用HPLC-DAD检测与交替惩罚三线性分解(APTLD)算法相结合对牛奶中的磺胺类兽药残留量进行了分析测定。尽管样品中组分分离不完全,并且存在大量干扰组分,但利用化学计量学二阶校正方法的“二阶优势”,仍能对该体系中感兴趣的磺胺组分给出准确的定量分析结果。
Chemometrics is a developing composite discipline of chemistry. The main focus of chemometrics is on applying the methods of mathematics, statistics and computer sciences to extracting chemical information, to designing the optimal scheme for chemical measurements and to elucidating the data collected from chemical measurements.
The second-order calibration methodologies can deal with some traditional difficult problems because of the second-order advantage. The chemometric methodologies coupled with higher-order analytical instruments can improve or replace the“chemical separation”with“mathematical separation”, enable accurate and reliable determination of the analyte concentrations even in the presence of uncalibrated interferents.
In this paper, the authors utilized the analytical instruments such as EEMs and HPLC-DAD, coupled with second-order calibration methodologies, and did some work in the research of complex multi-component systems. Studies presented in the thesis primarily deals with the following aspects:
In Chapter 2, it proposed a new approach for direct determination of arctiin content in plasma samples as well as a Chinese medicine (Arctium lappa L.) by the combination of excitation-emission matrix fluorescence and second-order calibration methods based on the parallel factor analysis (PARAFAC) and the alternating normalization-weighted error (ANWE) algorithms. The estimated content of arctiin in arctium lappa L. obtained by fluorescence determination was also satisfactory compared with that of the HPLC method. It can be seen that the suggested methods can be employed to directly determine arctiin, even in the presence of unknown and un-calibrated interferences, only with a simple pretreatment procedure.
The rhubarb is one of the most popular traditional Chinese herbal medicines. The main active constituents of rhubarb have been reported to be anthraquinones, such as emodin and chrysophanol. In Chapter 3, it was tried to use three-way excitation-emission matrix fluorescence combining chemometrics second-order calibration algorithms, including the alternating penalty trilinear decomposition (APTLD) algorithm and the alternating normalizationweigh (ANWE) algorithm, to determined emodin and chrysophanol even in presence of urine background interferents. Though the peaks of the analytes were heavily overlapped and urine background interferents coeluted with the compounds studied, good resolved results could be obtained. But it is a pity that the estimated content of the emodin is not acceptable, it maybe owe to the reaction of the emodin with the urin background interferents and then the fluorescence of emodin had been decreased. Thus, it only can obtained satisfactory estimated results of the chrysophanol in the urine by using the method mentioned.
In Chapter 4, HPLC-DAD coupled with chemometric second-order calibration method based on ATLD algorithm was applied toβ-adrenergic receptor-blocking agent in body fluids. Though the chromatographic and spectral peaks of the analytes were heavily overlapped and interferents coeluted with the compounds studied, good recoveries of the analytes could be obtained.
Sulfonamides constitute a group of drugs which are widely used in veterinary. Their metabolism process are slow in animal body, thus, residues of these drugs may remain in food of animal origin. In Chapter 5, a new method based on the use of HPLC-DAD coupled with the alternating penalty trilinear decomposition (APTLD) algorithm was applied to the rapid determination of sulfonamides in milk samples. Though the chromatographic and spectral peaks of the components were highly overlapped, good quantitative results could be obtained owing to the second order advantage. The application of second-order calibration methodologies provides a new technique to food analysis.
引文
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