新型分散液液微萃取技术用于环境及生物样品中痕量有害物质的分析
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摘要
分散液液微萃取技术(DLLME),作为一种新型液相微萃取模式,具有操作简单、快速、高效等优点,受到分析工作者的高度关注。因其在萃取剂、分散方式、联用技术等方面的快速发展,目前已被广泛用于不同基质样品中不同分析对象的分析。本文从萃取剂及已有方法的应用范围两方面做了相关工作,目的在于拓宽萃取剂的选择范围及扩大已有方法的应用范围,建立更多用于实际样品分析的有效方法。
本论文主要内容如下：
1.建立了[C6MIM][PF6]离子液体超声辅助分散液液微萃取/高效液相色谱测定水样和鱼样中孔雀石绿的新方法。在优化的萃取条件下,方法的检测限(按3σ)为0.005ng mL-1,精密度(RSD)为8.9%(C=0.5ng mL-1, n=3),富集倍数可达220。该方法用于实际样品的测定得到了满意的结果。与用于测定孔雀石绿的其他方法相比,该方法具有检测限低、萃取时间短、溶剂用量少、环境友好等特点。
2.以新型绿色溶剂-[Allylmim][PF6]离子液体作为萃取剂,建立了温控离子液体分散液液微萃取-高效液相色谱法用于同时测定水样中的四种酚类物质(2-氯酚、4-氯酚、双酚A、4-叔丁基酚)。在优化的萃取条件下,方法的检测限为0.55-1.7ng mL-1,精密度为2.2-5.4%(C=100ng mL-1)。用于实际样品的测定,加标回收率在92.3-102.7%之间。本方法与文献中报道的温控分散液液微萃取方法相比,两相更易分离。
3.建立了溶剂终止分散液液微萃取/气相色谱法用于水样中多环芳香烃的测定,扩大了溶剂终止分散液液微萃取方法的应用范围。在优化的萃取条件下,方法的检测限范围是0.52-5.11μL-1,用于实际样品的测定,加标回收率为80.2-115.1%。该方法与传统的分散液液微萃取相比,具有操作简单、快速的特点。
4.建立了基于重质溶剂的溶剂终止分散液液微萃取-高效液相色谱测定水样中甲基对硫磷的新方法。在优化的萃取条件下,方法的检测限是0.03 ng mL-1,精密度为3.3%(C=10 ng mL-1, n=3)。用于实际水样的测定,加标回收率在73.9-84.8%之间。本方法与常规分散液液微萃取相比,无需离心步骤,具有操作简单、快速等优点,可望用于野外环境水样中甲基对硫磷的原地处理。
Dispersive liquid-liquid microextraction(DLLME), an alternative mode of liquid phase microextraction(LPME), which shows remarkable attributes of simplicity, rapidity and high efficiency, has arisen much attention in analytical chemistry in recent years. With the rapid development of its agents in the extraction, the decentralized approach and the technical aspects combined, DLLME has been widely used for the analysis of different objects and different media samples. Some related work have been done in this article from the extraction agent and application of existing methods, which aimed at broadening the choice of extractant and expanding the scope of application of existing methods, developing more effective method for real sample analysis.
The major contents were summarized as follows.
1. A method of the ultrasound-assisted dispersive liquid-liquid microextraction with ionic liquid [C6mim][PF6] as extractant for the preconcentration of malachite green in fish and water samples was developed. Under the optimum conditions, the detection limit of MG as low as 0.005 ng mL-1 was obtained, while the relative standard deviation for three replication determination of 0.5 ng mL-1 was 8.9%. Enrichment factor can reach 220. The proposed method was applied successfully to the determination of MG in several samples. Compared with the traditional DLLME, this method presents a lower detection limit, shorter extraction time and less solvent.
2. A new method of temperature controlled [Allylmim][PF6]-based dispersive liquid-liquid microextraction with HPLC for the determination of 2-chlorophenol, p-chlorophenol,4-tert-butylphenol, bisphenol A in water samples was established. Under the optimum conditions, the detection limit of phenols was in the range of 0.55-1.7 ng mL-1 and relative standard deviation for three replication determination of 100 ng mL-1 was 2.2-5.4%. The proposed method was applied to the determination of phenols in Mineral water and the recoveries of spiked samples were in the range of 92.3-102.7%. Compared with the traditional TCIL-DLLME, the separation of two Phases became much easier in this method.
3. A new method was developed for the determination of PAHs in water samples using low-density extraction solvent-based solvent terminated dispersive liquid-liquid microextraction(ST-DLLME) followed by gas chromatography. Under the optimum conditions, the detection limit of PAHs was in the range of 0.52-5.11 ng mL-1. The proposed method was successfully applied to the determination of PAHs in environmental water samples and the recoveries of spiked samples were in the range of 80.2-115.1%. Compared with the traditional DLLME, this method offered significant advantages of simple operating and time saving.
4 A simple and fast method of solvent terminated dispersive liquid-liquid microextraction(ST-DLLME) was developed for the determination of methyl parathion (MP) in the water samples by high performance liquid chromatography(HPLC). Under the optimized conditions, the limit of detection of the method was 0.03 ng mL-1 and the precision(RSD) was 3.3% for the determination of 10 ng mL-1 MP(n=3). The proposed method was applied to the determination of MP in Yangtze River, East Lake and tap water samples with satisfied results. Comparing with traditional DLLME, it offered significant advantages of simple operating and taime saving (no centrifugation). And it is expected to be used for the situ treatment of methyl parathion in field and shows a good prospect in the rapid detection of trace residues of pesticides.
本论文主要内容如下：
1.建立了[C6MIM][PF6]离子液体超声辅助分散液液微萃取/高效液相色谱测定水样和鱼样中孔雀石绿的新方法。在优化的萃取条件下,方法的检测限(按3σ)为0.005ng mL-1,精密度(RSD)为8.9%(C=0.5ng mL-1, n=3),富集倍数可达220。该方法用于实际样品的测定得到了满意的结果。与用于测定孔雀石绿的其他方法相比,该方法具有检测限低、萃取时间短、溶剂用量少、环境友好等特点。
2.以新型绿色溶剂-[Allylmim][PF6]离子液体作为萃取剂,建立了温控离子液体分散液液微萃取-高效液相色谱法用于同时测定水样中的四种酚类物质(2-氯酚、4-氯酚、双酚A、4-叔丁基酚)。在优化的萃取条件下,方法的检测限为0.55-1.7ng mL-1,精密度为2.2-5.4%(C=100ng mL-1)。用于实际样品的测定,加标回收率在92.3-102.7%之间。本方法与文献中报道的温控分散液液微萃取方法相比,两相更易分离。
3.建立了溶剂终止分散液液微萃取/气相色谱法用于水样中多环芳香烃的测定,扩大了溶剂终止分散液液微萃取方法的应用范围。在优化的萃取条件下,方法的检测限范围是0.52-5.11μL-1,用于实际样品的测定,加标回收率为80.2-115.1%。该方法与传统的分散液液微萃取相比,具有操作简单、快速的特点。
4.建立了基于重质溶剂的溶剂终止分散液液微萃取-高效液相色谱测定水样中甲基对硫磷的新方法。在优化的萃取条件下,方法的检测限是0.03 ng mL-1,精密度为3.3%(C=10 ng mL-1, n=3)。用于实际水样的测定,加标回收率在73.9-84.8%之间。本方法与常规分散液液微萃取相比,无需离心步骤,具有操作简单、快速等优点,可望用于野外环境水样中甲基对硫磷的原地处理。
Dispersive liquid-liquid microextraction(DLLME), an alternative mode of liquid phase microextraction(LPME), which shows remarkable attributes of simplicity, rapidity and high efficiency, has arisen much attention in analytical chemistry in recent years. With the rapid development of its agents in the extraction, the decentralized approach and the technical aspects combined, DLLME has been widely used for the analysis of different objects and different media samples. Some related work have been done in this article from the extraction agent and application of existing methods, which aimed at broadening the choice of extractant and expanding the scope of application of existing methods, developing more effective method for real sample analysis.
The major contents were summarized as follows.
1. A method of the ultrasound-assisted dispersive liquid-liquid microextraction with ionic liquid [C6mim][PF6] as extractant for the preconcentration of malachite green in fish and water samples was developed. Under the optimum conditions, the detection limit of MG as low as 0.005 ng mL-1 was obtained, while the relative standard deviation for three replication determination of 0.5 ng mL-1 was 8.9%. Enrichment factor can reach 220. The proposed method was applied successfully to the determination of MG in several samples. Compared with the traditional DLLME, this method presents a lower detection limit, shorter extraction time and less solvent.
2. A new method of temperature controlled [Allylmim][PF6]-based dispersive liquid-liquid microextraction with HPLC for the determination of 2-chlorophenol, p-chlorophenol,4-tert-butylphenol, bisphenol A in water samples was established. Under the optimum conditions, the detection limit of phenols was in the range of 0.55-1.7 ng mL-1 and relative standard deviation for three replication determination of 100 ng mL-1 was 2.2-5.4%. The proposed method was applied to the determination of phenols in Mineral water and the recoveries of spiked samples were in the range of 92.3-102.7%. Compared with the traditional TCIL-DLLME, the separation of two Phases became much easier in this method.
3. A new method was developed for the determination of PAHs in water samples using low-density extraction solvent-based solvent terminated dispersive liquid-liquid microextraction(ST-DLLME) followed by gas chromatography. Under the optimum conditions, the detection limit of PAHs was in the range of 0.52-5.11 ng mL-1. The proposed method was successfully applied to the determination of PAHs in environmental water samples and the recoveries of spiked samples were in the range of 80.2-115.1%. Compared with the traditional DLLME, this method offered significant advantages of simple operating and time saving.
4 A simple and fast method of solvent terminated dispersive liquid-liquid microextraction(ST-DLLME) was developed for the determination of methyl parathion (MP) in the water samples by high performance liquid chromatography(HPLC). Under the optimized conditions, the limit of detection of the method was 0.03 ng mL-1 and the precision(RSD) was 3.3% for the determination of 10 ng mL-1 MP(n=3). The proposed method was applied to the determination of MP in Yangtze River, East Lake and tap water samples with satisfied results. Comparing with traditional DLLME, it offered significant advantages of simple operating and taime saving (no centrifugation). And it is expected to be used for the situ treatment of methyl parathion in field and shows a good prospect in the rapid detection of trace residues of pesticides.
引文
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