固相吸附剂在固体样品处理中的应用
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摘要
根据对国内外烟草和中草药安全检测中各种问题的分析以及对目前烟草和中草药的安全总趋势的阐述，本文介绍了不同类型的固相吸附剂及其吸附机理和应用。以烟草和中草药作为研究对象，将不同固相吸附剂应用于改进的QuEChERS（Quick、Easy、Cheap、Effective、Rugged、Safe）预处理技术和基质固相分散（MSPD）技术，结合气相色谱-质谱法（GC-MS）和超快速液相色谱（UFLC），对不同性质的固体样品的分析进行了研究。
一、将硅藻土应用于同时萃取、分离、测定栀子中栀子苷的MSPD-UFLC方法中。对各项实验参数，包括固相吸附剂的种类、洗脱剂的种类、洗脱剂的体积、固相吸附剂与样品的质量比以及样品的粒径，通过单因素水平实验和正交试验设计法对实验条件进行了优化。对方法的一系列性能指标进行了研究，并对实际样品进行了分析，并将其与其它传统方法进行了对比。
二、将硅胶应用在萃取中草药丹参根部的苏丹红染料的MSPD萃取方法中，UFLC用于测定这些待测物。对影响MSPD的一些实验参数通过优化得到最优的条件。对方法的一系列性能指标等进行了考察，最后将MSPD-UFLC分析方法应用于五种不同产地的丹参实际样品中染料的测定。
三、将改进的QuEChERS预处理方法与GC-MS联用，在选择离子检测模式（SIM）下提取和检测了烟草中六种拟除虫菊酯类杀虫剂残留。将烟草中拟除虫菊酯类杀虫剂快速提取和净化结合起来，通过乙腈-饱和氯化钠水溶液双水相混合萃取、N-丙基乙二胺（PSA）键合硅胶作为固相吸附剂净化，建立了一个高效、快速的测定烟草中拟除虫菊酯类杀虫剂残留的新方法。
四、将中性三氧化二铝应用于烟草中三嗪类除草剂残留萃取中。通过将MSPD和超快速液相色谱-紫外检测器（UFLC-UV）进行联用，建立并验证了一种实用、经济的检测烟草中三嗪类除草剂残留的新方法。对影响三嗪类除草剂检测结果的各项实验参数，包括三嗪类除草剂检测波长、固相吸附剂的种类和质量、洗脱剂的性质和体积、固相吸附剂与样品的质量比等因素，通过单因素水平实验和正交试验设计法进行了优化，并进行了相应的方法学考察和验证。
Throughout the history, tobacco and Chinese herbal medicine have always beenan important part of the human daily necessities. In daily life, shoddy tobacco andChinese herbal medicine cause consumers in economic losses at the same time, moreimportance is the direct threat to the health and safety of consumers. In order toguarantee the tobacco and Chinese herbal medicine safety, the law must be enforcedto restrain manufacturers and the quality supervision for tobacco and Chinese herbalmedicine conducted various stages from planting to product is needed. Analysis of thesample is an important mean of quality supervision. With the continuous progress ofscience and technology and cross discipline, many new extraction and separationtechniques have been developed, which improves conditions for the safetysupervision of tobacco and Chinese herbal medicine. Based on the type of the sampleand the property of the target compounds, suitable pretreatment method should beapplied to eliminate the interferences or make the interferences content decrease.Sample pre-treatment method can affect, not only on the cost of sample testing andprocessing environment, but also on the speed and quality of sample pretreatment.The speed and accuracy of analysis of sample also is related to the sample treatmentmethod.
In this thesis, tobacco and Chinese herbal medicine were used as the samples,different solid sorbents were used to treat solid samples by using the modifiedQuEChERS and matrix solid-phase dispersion (MSPD).
1. Celite was used as the dispersing adsorbent and used in MSPD-fast liquidchromatography (UFLC) for the simultaneous extraction, separation anddetermination of geniposide from the fruit of Gardenia jasminoides Ellis. Theexperiment parameters, including type of dispersing sorbent and elution solvent,volume of elution solvent, ratio of sorbent to sample and particle size of sample wereoptimized by univariate method and orthogonal screening. The feasibility of themethod was evaluated by investigating linearity, precision, limit of decetion (LOD)and limit of quantitation (LOQ), and analyzing real sample. LOD and LOQ were0.026and0.087μg mL-1, respectively. The intra-and inter-day precision ranged from0.6%to3.9%. Compared with the conventional extraction methods, such as UAE andSE, the present method is quicker and more effective.
2. Silica gel was used as the dispersing sorbent in MSPD extraction of Sudandyes from the roots of Salvia miltiorrhiza Bge.. UFLC was applied to thedetermination of the analytes. The experimental parameters affecting MSPD wereoptimized, such as dispersing sorbent type, the ratio of sorbent to sample, washingsolvent type and elution solvent type. The analytical performances are satisfactory.LODs obtained by the present method were in the range of0.013-0.024μg g-1, andtwenty times lower than the maximum residue limits (MRLs) established by Europeanregulations. The recoveries at three spiked levels (0.1,1.0,5.0μg g-1) were between80.6%and96.1%with RSDs ranging from2.3%to8.6%.
3. The extraction and determination of six pyrethroid pesticide residues intobacco by a modifed QuEChERS sample preparation procedure and GC-MS-SIMwas developed. Methyl cyanide (MeCN)-saturated salt aqueous was used as theaqueous two-phase extraction solvent, and N-propylethylenediamine (PSA) waschosen as the clean-up sorbent. The extraction was coupled with clean-up forextraction of pyrethroid pesticides in tobacco. The time, labor and reagentconsumption were reduced. The results showed quite good analytical performances interms of the linearity, sensitivity and repeatability. The LODs obtained by the presentmethod were much lower than the guidance residue levels (GRLs) regulated by theAgrochemical Advisory Committee of CORESTA, an association of organizations for scientific research of tobacco. The developed method is suitable for routine analysisof tobacco and tobacco products.
4. Alumina-N was used as the dispersing sorbent in the extraction of triazineherbicides in tobacco. Based on the MSPD extraction and UFLC-UV detection, apractical, economical MSPD-UFLC method for the determination of seven triazineherbicides in tobacco has been established. The experiment parameters, includingwavelength of triazine herbicides, type of dispersing sorbent and elution solvent,volume of elution solvent, and ratio of sorbent to sample were optimized by univariatemethod and orthogonal screening. The feasibility of the method was evaluated byinvestigating linearity, accuracy, precision, LOD and LOQ and analyzing real sampleanalysis. The LOD and LOQ were in the range of1.38-6.41μg kg-1and4.61-21.4μgkg-1, respectively. The recoveries ranged from91.1%to117.1%. The intra-day andinter-day RSDs obtained were in the range of1.2%-6.7%and0.9%-7.5%, respectively.This method has potential to be applied for the determination of trace residues incomplicated plant materials by varying the extraction conditions.
一、将硅藻土应用于同时萃取、分离、测定栀子中栀子苷的MSPD-UFLC方法中。对各项实验参数，包括固相吸附剂的种类、洗脱剂的种类、洗脱剂的体积、固相吸附剂与样品的质量比以及样品的粒径，通过单因素水平实验和正交试验设计法对实验条件进行了优化。对方法的一系列性能指标进行了研究，并对实际样品进行了分析，并将其与其它传统方法进行了对比。
二、将硅胶应用在萃取中草药丹参根部的苏丹红染料的MSPD萃取方法中，UFLC用于测定这些待测物。对影响MSPD的一些实验参数通过优化得到最优的条件。对方法的一系列性能指标等进行了考察，最后将MSPD-UFLC分析方法应用于五种不同产地的丹参实际样品中染料的测定。
三、将改进的QuEChERS预处理方法与GC-MS联用，在选择离子检测模式（SIM）下提取和检测了烟草中六种拟除虫菊酯类杀虫剂残留。将烟草中拟除虫菊酯类杀虫剂快速提取和净化结合起来，通过乙腈-饱和氯化钠水溶液双水相混合萃取、N-丙基乙二胺（PSA）键合硅胶作为固相吸附剂净化，建立了一个高效、快速的测定烟草中拟除虫菊酯类杀虫剂残留的新方法。
四、将中性三氧化二铝应用于烟草中三嗪类除草剂残留萃取中。通过将MSPD和超快速液相色谱-紫外检测器（UFLC-UV）进行联用，建立并验证了一种实用、经济的检测烟草中三嗪类除草剂残留的新方法。对影响三嗪类除草剂检测结果的各项实验参数，包括三嗪类除草剂检测波长、固相吸附剂的种类和质量、洗脱剂的性质和体积、固相吸附剂与样品的质量比等因素，通过单因素水平实验和正交试验设计法进行了优化，并进行了相应的方法学考察和验证。
Throughout the history, tobacco and Chinese herbal medicine have always beenan important part of the human daily necessities. In daily life, shoddy tobacco andChinese herbal medicine cause consumers in economic losses at the same time, moreimportance is the direct threat to the health and safety of consumers. In order toguarantee the tobacco and Chinese herbal medicine safety, the law must be enforcedto restrain manufacturers and the quality supervision for tobacco and Chinese herbalmedicine conducted various stages from planting to product is needed. Analysis of thesample is an important mean of quality supervision. With the continuous progress ofscience and technology and cross discipline, many new extraction and separationtechniques have been developed, which improves conditions for the safetysupervision of tobacco and Chinese herbal medicine. Based on the type of the sampleand the property of the target compounds, suitable pretreatment method should beapplied to eliminate the interferences or make the interferences content decrease.Sample pre-treatment method can affect, not only on the cost of sample testing andprocessing environment, but also on the speed and quality of sample pretreatment.The speed and accuracy of analysis of sample also is related to the sample treatmentmethod.
In this thesis, tobacco and Chinese herbal medicine were used as the samples,different solid sorbents were used to treat solid samples by using the modifiedQuEChERS and matrix solid-phase dispersion (MSPD).
1. Celite was used as the dispersing adsorbent and used in MSPD-fast liquidchromatography (UFLC) for the simultaneous extraction, separation anddetermination of geniposide from the fruit of Gardenia jasminoides Ellis. Theexperiment parameters, including type of dispersing sorbent and elution solvent,volume of elution solvent, ratio of sorbent to sample and particle size of sample wereoptimized by univariate method and orthogonal screening. The feasibility of themethod was evaluated by investigating linearity, precision, limit of decetion (LOD)and limit of quantitation (LOQ), and analyzing real sample. LOD and LOQ were0.026and0.087μg mL-1, respectively. The intra-and inter-day precision ranged from0.6%to3.9%. Compared with the conventional extraction methods, such as UAE andSE, the present method is quicker and more effective.
2. Silica gel was used as the dispersing sorbent in MSPD extraction of Sudandyes from the roots of Salvia miltiorrhiza Bge.. UFLC was applied to thedetermination of the analytes. The experimental parameters affecting MSPD wereoptimized, such as dispersing sorbent type, the ratio of sorbent to sample, washingsolvent type and elution solvent type. The analytical performances are satisfactory.LODs obtained by the present method were in the range of0.013-0.024μg g-1, andtwenty times lower than the maximum residue limits (MRLs) established by Europeanregulations. The recoveries at three spiked levels (0.1,1.0,5.0μg g-1) were between80.6%and96.1%with RSDs ranging from2.3%to8.6%.
3. The extraction and determination of six pyrethroid pesticide residues intobacco by a modifed QuEChERS sample preparation procedure and GC-MS-SIMwas developed. Methyl cyanide (MeCN)-saturated salt aqueous was used as theaqueous two-phase extraction solvent, and N-propylethylenediamine (PSA) waschosen as the clean-up sorbent. The extraction was coupled with clean-up forextraction of pyrethroid pesticides in tobacco. The time, labor and reagentconsumption were reduced. The results showed quite good analytical performances interms of the linearity, sensitivity and repeatability. The LODs obtained by the presentmethod were much lower than the guidance residue levels (GRLs) regulated by theAgrochemical Advisory Committee of CORESTA, an association of organizations for scientific research of tobacco. The developed method is suitable for routine analysisof tobacco and tobacco products.
4. Alumina-N was used as the dispersing sorbent in the extraction of triazineherbicides in tobacco. Based on the MSPD extraction and UFLC-UV detection, apractical, economical MSPD-UFLC method for the determination of seven triazineherbicides in tobacco has been established. The experiment parameters, includingwavelength of triazine herbicides, type of dispersing sorbent and elution solvent,volume of elution solvent, and ratio of sorbent to sample were optimized by univariatemethod and orthogonal screening. The feasibility of the method was evaluated byinvestigating linearity, accuracy, precision, LOD and LOQ and analyzing real sampleanalysis. The LOD and LOQ were in the range of1.38-6.41μg kg-1and4.61-21.4μgkg-1, respectively. The recoveries ranged from91.1%to117.1%. The intra-day andinter-day RSDs obtained were in the range of1.2%-6.7%and0.9%-7.5%, respectively.This method has potential to be applied for the determination of trace residues incomplicated plant materials by varying the extraction conditions.
引文
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