加速溶剂萃取和离子液体微萃取在土壤样品处理中的应用
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摘要
论文采用加速溶剂萃取和离子液体微萃取法研究了土壤样品中农药和邻苯二甲酸酯的萃取，通过对加速溶剂萃取条件的优化和对离子液体微萃取方法改进以及条件优化，建立了一些对复杂土壤样品的更快速、高效、操作简便且环保的前处理方法。论文研究的主要萃取方法有微波辅助离子液体均匀萃取、加速溶剂萃取和超声辅助离子液体微萃取法。
用微波辅助-离子液体均匀萃取-高效液相色谱法测定土壤样品中的烯酰吗啉、苯噻酰草胺、稻瘟灵和恶草酮。该法首先将水和亲水性离子液体同时添加到土壤样品中，经过微波辅助萃取，再加入离子对试剂六氟磷酸铵，该离子对试剂的阴离子与亲水性离子液体的阳离子形成新的疏水性六氟磷酸盐离子液体，同时待测物被富集到新生成的离子液体相中，得到分离。该方法通过不同性质的离子液体之间的转化，使得对土壤样品中农药残留的萃取更简单、快速。
用加速溶剂萃取-高效液相色谱串联质谱法测定土壤样品中的九种农药残留，用此法对环境土壤样品进行了分析，并与振荡萃取法和索氏提萃取法进行了比较，实验结果表明，该方法萃取回收率高、溶剂消耗较少、萃取速度快、自动化高、操作安全可靠。
用加速溶剂萃取-高效液相色谱串联质谱法，并采用大气压化学电离源对土壤样品中十一种邻苯二甲酸酯进行测定。与索氏萃取法和超声萃取法进行了比较，实验结果表明，该方法可以获得较高的回收率和较低的检出限，由于该方法可以达到较高的萃取温度，萃取效果更好、干扰更小、省时、省溶剂。
采用超声辅助-离子液体微萃取-高效液相色谱法测定土壤样品中磺酰脲类除草剂。超声辅助萃取是利用超声波在萃取过程中产生的强烈空化效应等多级效应，来加快萃取过程中的传质作用，从而提高萃取效率。该实验方法操作简单、快速、无污染。
In the determination of organic pollutants in soil samples, sample preparation is veryimportant, because the matrix is complicated and concentration of analyte is very low. It isimportant to develop fast, efficient, simple and green sample preparation method in orderto obtain reliable, repeatable analytical result.
Dispersive liquid liquid microextraction(DLLME), which is a new mode of liquidphase microextraction, was proposed recently. In this method, the appropriate extractionsolvent and dispersant was injected into the aqueous sample rapidly with syringe, followedby oscillation, ultrasoud or microwave extraction. The extraction solvent was dispersedinto the aqueous sample as very fine droplets and the analytes were easily and fasttransferred to the extraction solvent. When extraction equilibrium was obtained, phaseseparation was performed by centrifugation, and the enriched analytes in the sedimentphase were determined by chromatographic methods. In this method, extraction,enrichment and separation were carried out at the same time. The advantages of theDLLME are simple, rapid, enviromental friendly, inexpensive and highly efficient. Theapplication of DLLME in trace analysis is wide.
Accelerated solvent extraction is a new solvent extraction method, and can be appliedto the treatment of a solid or semi-solid samples. The extraction efficiency and extractionspeed are improved by improving the extraction temperature and pressure. The solutbiltyand diffusion rate increased with the elevated temperature and pressure, so the efficiencyof extraction. The method has some advantages, such as low envriomental pollution, lowexpenditure of organic solvent, rapidity, high recovery and automation.
The room temperature ionic liquids (RTILs) are promising green solvents and were applied to the extraction and separation. The RTIL has some unique chemical and physicalproperties, such as nonvolatility, good thermal stability, superior solutility and tunableproperties. The extraction should be enviromental friendly because volatile organicsolvents are replaced by RTIL.
In this thesis, soil was taken as analytical sample. The pesticides and phthalic acidesters were extracted and determined by accelerated solvent extraction-liquidchromatography tadem mass spectrometry and ionic liquid microextraction-liquidchromatography.
The microwave-assisted homogeneous ionic liquid microextraction (MA-HILME)coupled with high-performance liquid chromatogrophy, was developed for determinationof dimethomorph, mefenacet, isoprothiolane, oxadiazon. Some experimental parameters,such as type of IL, microwave power, microwave time, sample amount, IL volume,ionic-pairing agent amount, time of centrifugation were examined. The recoveries from74.2～97.9%were obtained for three samples at fortification levels (35ng·g-1and140ng·g-1) with relative standard deviations (RSDs)≤5.97%. Compared with ultrasonic andSoxhlet extraction, there is little difference in recoveries obtained by the three methods,only a small amount of IL(0.10mL) was used in the present method. The extraction timeof the present method(16min) was shorter than those of UE(40min) and SE(240min).The present method was a comparatively satisfactory method.
A rapid and accurate method based on accelerated solvent extraction liquidchromatography tandem mass spectrometry(LC-MS/MS) was developed for thedetermination of carbofuran, dimethomorph, mefenacet, isoprothiolane, acetochlor,pretilachlor, uizalofop, oxadiazon and fenpropathrin in soil. Some experimentalparameters, such as extraction solvent, extraction temperature, cycle number, static time,flush volume, purging time, were examined and optimized. The analytes were extracted byaccelerated solvent extraction using acetonitrile as the extraction solvent. The recoveriesfrom90.0～105.0%were obtained for five samples at fortification levels (10ng·g-1and100ng·g-1) with relative standard deviations (RSDs)in1.0～5.9%. Compared withoscillating and Soxhlet extraction, this method is more rapid and suitable to the extractionof pesticides in soil.
The determination of11phthalic acid esters(PAEs) in soil sample by acceleratedsolvent extraction coupled with liquid chromatography tandem mass sepctrometricdetection was described. The1.0g sample was used. n-Hexane was used as the extractionsolvent. The extraction conditions, such as extraction temperature, cycle number, staticVI time, flush volume, purging time were160℃,4,12min,60%,90s, respctively. Thismethod is rapid, sensitive and suitable to the determination of PAEs in soil. Theorthogonal test was preformed and the results match the results obtained by single factorexperiment. The range analysis indicated that the extraction temperature was the maininfluence factor. The recoveries of11phthalic acid esters were between72.8～101.8%,with relative standard deviations (RSDs) between1.7～6.7%. Compared with Soxhletand ultrasonic extraction, higher recovery and lower limit of detection were obtained bythis method.
The ultrasound-assisted ionic liquid microextraction coupled with high-performanceliquid chromatographic detection, has been developed for determination of sulfonylureaherbicides. The key parameters, such as type of IL, volume of IL, amount of sample,ultrasonic power and time, were examined and optimized. The Recoveries of nicosulfuron,metsulfuron-methyl, bensulfuron-methyl, pyrazosulfuron-ethyl are94.1～99.4%(RSD≤6.32%）,81.1～92.2%(RSD≤5.41%),81.3～90.6%(RSD≤3.61%),93.6～100.1%(RSD≤7.44%) and the limits of detection are10.2,11.3,8.5and7.7ng·g-1, respectively.The intra-day and inter-day RSD are lower than7.56%and7.93%, respectively.Compared with Soxhlet and ultrasonic extraction, the present method is easier operated,more rapid and enviromental friendly.
用微波辅助-离子液体均匀萃取-高效液相色谱法测定土壤样品中的烯酰吗啉、苯噻酰草胺、稻瘟灵和恶草酮。该法首先将水和亲水性离子液体同时添加到土壤样品中，经过微波辅助萃取，再加入离子对试剂六氟磷酸铵，该离子对试剂的阴离子与亲水性离子液体的阳离子形成新的疏水性六氟磷酸盐离子液体，同时待测物被富集到新生成的离子液体相中，得到分离。该方法通过不同性质的离子液体之间的转化，使得对土壤样品中农药残留的萃取更简单、快速。
用加速溶剂萃取-高效液相色谱串联质谱法测定土壤样品中的九种农药残留，用此法对环境土壤样品进行了分析，并与振荡萃取法和索氏提萃取法进行了比较，实验结果表明，该方法萃取回收率高、溶剂消耗较少、萃取速度快、自动化高、操作安全可靠。
用加速溶剂萃取-高效液相色谱串联质谱法，并采用大气压化学电离源对土壤样品中十一种邻苯二甲酸酯进行测定。与索氏萃取法和超声萃取法进行了比较，实验结果表明，该方法可以获得较高的回收率和较低的检出限，由于该方法可以达到较高的萃取温度，萃取效果更好、干扰更小、省时、省溶剂。
采用超声辅助-离子液体微萃取-高效液相色谱法测定土壤样品中磺酰脲类除草剂。超声辅助萃取是利用超声波在萃取过程中产生的强烈空化效应等多级效应，来加快萃取过程中的传质作用，从而提高萃取效率。该实验方法操作简单、快速、无污染。
In the determination of organic pollutants in soil samples, sample preparation is veryimportant, because the matrix is complicated and concentration of analyte is very low. It isimportant to develop fast, efficient, simple and green sample preparation method in orderto obtain reliable, repeatable analytical result.
Dispersive liquid liquid microextraction(DLLME), which is a new mode of liquidphase microextraction, was proposed recently. In this method, the appropriate extractionsolvent and dispersant was injected into the aqueous sample rapidly with syringe, followedby oscillation, ultrasoud or microwave extraction. The extraction solvent was dispersedinto the aqueous sample as very fine droplets and the analytes were easily and fasttransferred to the extraction solvent. When extraction equilibrium was obtained, phaseseparation was performed by centrifugation, and the enriched analytes in the sedimentphase were determined by chromatographic methods. In this method, extraction,enrichment and separation were carried out at the same time. The advantages of theDLLME are simple, rapid, enviromental friendly, inexpensive and highly efficient. Theapplication of DLLME in trace analysis is wide.
Accelerated solvent extraction is a new solvent extraction method, and can be appliedto the treatment of a solid or semi-solid samples. The extraction efficiency and extractionspeed are improved by improving the extraction temperature and pressure. The solutbiltyand diffusion rate increased with the elevated temperature and pressure, so the efficiencyof extraction. The method has some advantages, such as low envriomental pollution, lowexpenditure of organic solvent, rapidity, high recovery and automation.
The room temperature ionic liquids (RTILs) are promising green solvents and were applied to the extraction and separation. The RTIL has some unique chemical and physicalproperties, such as nonvolatility, good thermal stability, superior solutility and tunableproperties. The extraction should be enviromental friendly because volatile organicsolvents are replaced by RTIL.
In this thesis, soil was taken as analytical sample. The pesticides and phthalic acidesters were extracted and determined by accelerated solvent extraction-liquidchromatography tadem mass spectrometry and ionic liquid microextraction-liquidchromatography.
The microwave-assisted homogeneous ionic liquid microextraction (MA-HILME)coupled with high-performance liquid chromatogrophy, was developed for determinationof dimethomorph, mefenacet, isoprothiolane, oxadiazon. Some experimental parameters,such as type of IL, microwave power, microwave time, sample amount, IL volume,ionic-pairing agent amount, time of centrifugation were examined. The recoveries from74.2～97.9%were obtained for three samples at fortification levels (35ng·g-1and140ng·g-1) with relative standard deviations (RSDs)≤5.97%. Compared with ultrasonic andSoxhlet extraction, there is little difference in recoveries obtained by the three methods,only a small amount of IL(0.10mL) was used in the present method. The extraction timeof the present method(16min) was shorter than those of UE(40min) and SE(240min).The present method was a comparatively satisfactory method.
A rapid and accurate method based on accelerated solvent extraction liquidchromatography tandem mass spectrometry(LC-MS/MS) was developed for thedetermination of carbofuran, dimethomorph, mefenacet, isoprothiolane, acetochlor,pretilachlor, uizalofop, oxadiazon and fenpropathrin in soil. Some experimentalparameters, such as extraction solvent, extraction temperature, cycle number, static time,flush volume, purging time, were examined and optimized. The analytes were extracted byaccelerated solvent extraction using acetonitrile as the extraction solvent. The recoveriesfrom90.0～105.0%were obtained for five samples at fortification levels (10ng·g-1and100ng·g-1) with relative standard deviations (RSDs)in1.0～5.9%. Compared withoscillating and Soxhlet extraction, this method is more rapid and suitable to the extractionof pesticides in soil.
The determination of11phthalic acid esters(PAEs) in soil sample by acceleratedsolvent extraction coupled with liquid chromatography tandem mass sepctrometricdetection was described. The1.0g sample was used. n-Hexane was used as the extractionsolvent. The extraction conditions, such as extraction temperature, cycle number, staticVI time, flush volume, purging time were160℃,4,12min,60%,90s, respctively. Thismethod is rapid, sensitive and suitable to the determination of PAEs in soil. Theorthogonal test was preformed and the results match the results obtained by single factorexperiment. The range analysis indicated that the extraction temperature was the maininfluence factor. The recoveries of11phthalic acid esters were between72.8～101.8%,with relative standard deviations (RSDs) between1.7～6.7%. Compared with Soxhletand ultrasonic extraction, higher recovery and lower limit of detection were obtained bythis method.
The ultrasound-assisted ionic liquid microextraction coupled with high-performanceliquid chromatographic detection, has been developed for determination of sulfonylureaherbicides. The key parameters, such as type of IL, volume of IL, amount of sample,ultrasonic power and time, were examined and optimized. The Recoveries of nicosulfuron,metsulfuron-methyl, bensulfuron-methyl, pyrazosulfuron-ethyl are94.1～99.4%(RSD≤6.32%）,81.1～92.2%(RSD≤5.41%),81.3～90.6%(RSD≤3.61%),93.6～100.1%(RSD≤7.44%) and the limits of detection are10.2,11.3,8.5and7.7ng·g-1, respectively.The intra-day and inter-day RSD are lower than7.56%and7.93%, respectively.Compared with Soxhlet and ultrasonic extraction, the present method is easier operated,more rapid and enviromental friendly.
引文
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