磁性石墨烯復合材料在蔬菜保鮮劑檢測中的應用研究
發(fā)布時間：2019-04-20 16:27
【摘要】：保鮮劑通常用于蔬菜的保鮮,以防止其腐爛變質。而大多數的化學保鮮劑為農藥,在使用過程中出現亂用、濫用、殘留量超標等現象,已經嚴重威脅到消費者的身體健康。在食品安全越來越受到關注的情況下,尋求一種安全有效的除雜吸附劑用于樣品前處理技術顯得尤為重要。磁性納米材料(Fe_3O_4)具有超順磁性,在外加磁場的作用下可快速從溶液中分離。在分析檢測中,利用其比表面積大和毒性低的優(yōu)點,再將其與其他材料結合,可望提高提取效率和分離速度。石墨烯(G)是由碳原子以sp2雜化形成的只有一層原子厚度的二維晶體,具有超大的比表面積,大的共軛體系,能夠耐酸、耐堿、耐熱。在G的表面可進行功能化修飾以產生不同的作用效果。離子液體(IL)是由有機陽離子和無機或有機陰離子組成,在室溫附近呈液態(tài)的有機鹽類。IL因其具有熱穩(wěn)定性好、溶解能力強等優(yōu)良性能被廣泛應用于有機合成、催化、分離分析等領域。本文通過制備新型磁性石墨烯復合物作為凈化吸附材料實現蔬菜中多種保鮮劑快速有效的檢測。第一部分基于磁性石墨烯復合材料快速檢測蔬菜中16種保鮮劑目的:基于Qu ECh ERS方法的原理,制備Fe_3O_4@Si O2@G新型復合材料,將其作為磁性固相萃取(MSPE)的吸附劑快速凈化蔬菜樣品,通過氣相色譜質譜儀(GC-MS)同時檢測蔬菜樣品中16種保鮮劑。方法:采用化學鍵合法制備Fe_3O_4@Si O2@G,優(yōu)化合成比例,以蔬菜為原料經乙腈提取,Fe_3O_4@Si O2@G除雜凈化,用GC-MS外標法定量。結果:16種保鮮劑在0.02~2.00 mg/L范圍內線性關系良好,相關系數(R2)為0.9946~0.9998,檢測限(LOD)在0.21~11.50μg/kg之間,回收率為78.3%~116.7%,相對標準偏差為1.4%~11.9%。結論:本文制備的Fe_3O_4@Si O2@G具有良好的吸附能力和超順磁性,極大地提升了分離速度,檢測結果表明本方法具有快速、準確、靈敏度高等特點,能夠應用于實際蔬菜樣品中16種保鮮劑的測定。第二部分基于磁性石墨烯聚離子液體復合材料快速檢測蔬菜中20種保鮮劑目的:制備200~1000 nm的磁性納米粒(Fe_3O_4),合成Fe_3O_4@Si O2@G@PIL復合材料作為改進Qu ECh ERS法的吸附劑,結合氣相色譜質譜(GC-MS)分析,建立快速測定蔬菜中20種保鮮劑的方法。方法:通過化學沉淀法控制合成條件,制備了不同粒徑大小的Fe_3O_4,再分別制備不同粒徑大小的Fe_3O_4@Si O2@G@PIL復合材料。以蔬菜為原料,經正己烷飽和的乙腈提取,將不同粒徑的復合材料作為除雜吸附劑,并比較作用效果,用GC-MS外標法定量。結果:20種保鮮劑在0.02~2.00 mg/L呈現良好的線性,相關系數(R2)為0.9972~0.9999,檢測限為0.82~6.64μg/kg。結論:制備的Fe_3O_4@Si O2@G@PIL復合材料具有良好的吸附性能,可應用于蔬菜樣品中20種保鮮劑的高效快速檢測。
[Abstract]:Preservatives are usually used to keep vegetables fresh to prevent their decay. The majority of chemical preservatives are pesticides, which appear in the process of use, abuse, residue exceeding the standard and other phenomena, has seriously threatened the health of consumers. In the case of more and more attention to food safety, it is very important to find a safe and effective adsorbent for sample pretreatment. Magnetic nanomaterials (Fe_3O_4) are superparamagnetic and can be rapidly separated from the solution under the action of external magnetic field. By using the advantages of large specific surface area and low toxicity, and combining it with other materials, the extraction efficiency and separation speed can be improved. Graphene (G) is a two-dimensional crystal with only one layer of atom thickness formed by the hybridization of carbon atoms with sp2. It has a large specific surface area and a large conjugate system, which can withstand acid, alkali and heat resistance. Functionalized modification can be performed on the surface of G to produce different effects. Ionic liquid (IL) is composed of organic cations and inorganic or organic anions. Il is a liquid organic salt near room temperature. Il is widely used in organic synthesis and catalysis because of its excellent properties such as good thermal stability, strong solubility and so on. Separation analysis and other fields. In this paper, the preparation of new magnetic graphene complexes as purification adsorption materials to achieve rapid and effective detection of a variety of preservative in vegetables. The first part is based on the magnetic graphene composite rapid detection of 16 kinds of preservative in vegetables objective: based on the principle of Qu ECh ERS method, Fe_3O_4@Si O _ 2 / G composite material was prepared. It was used as an adsorbent for magnetic solid phase extraction of (MSPE) to purify vegetable samples rapidly. Sixteen preservative agents in vegetable samples were simultaneously determined by gas chromatography mass spectrometry (GC-MS). Methods: Fe_3O_4@Si O 2 / G was prepared by chemical bonding method. The ratio of synthesis was optimized. Vegetables were extracted with acetonitrile and cleaned up by Fe_3O_4@Si O 2? G, and quantified by external standard method of GC-MS. Results: the linear range of 16 preservatives was 0.02 ~ 2.00 mg/L, the correlation coefficient (R ~ 2) was 0.9946 渭 g / kg, the detection limit was 0.21 ~ 11.50 渭 g / kg, the recovery was 78.3% ~ 116.7%, the correlation coefficient was 0.9946 ~ 0.9998, the detection limit was 0.21 ~ 11.50 渭 g / kg, and the recovery was 78.3%. The relative standard deviation is 1.4% and 11.9%. Conclusion: the Fe_3O_4@Si O 2 G prepared in this paper has good adsorption ability and superparamagnetism, which greatly improves the separation speed. The detection results show that the method is rapid, accurate and sensitive. It can be applied to the determination of 16 kinds of preservative in actual vegetable samples. The second part is based on the rapid detection of 20 kinds of preservatives in vegetables based on magnetic graphene polyionic liquid composites. Objective: to prepare magnetic nanoparticles (Fe_3O_4) of 200 渭 1 000 nm. A rapid method for the determination of 20 preservative agents in vegetables was established by synthesizing Fe_3O_4@Si O2@G@PIL composites as adsorbents for improved Qu ECh ERS method combined with gas chromatography mass spectrometry (GC-MS). Methods: Fe_3O_4, composites with different particle sizes were prepared by chemical precipitation method, and then Fe_3O_4@Si O2@G@PIL composites with different particle sizes were prepared respectively. Using vegetables as raw materials and acetonitrile saturated with n-hexane, composite materials with different particle sizes were used as adsorbents for impurity removal. The effects were compared and quantified by GC-MS external standard method. Results: the calibration curves of 20 preservatives were linear at 0.02 ~ 2.00 mg/L, the correlation coefficient (R2) was 0.9972 渭 g / kg. and the detection limit was 0.82 ~ 6.64 渭 g / kg.. Conclusion: the prepared Fe_3O_4@Si O2@G@PIL composites have good adsorption properties and can be used for the rapid and efficient detection of 20 kinds of preservative in vegetable samples.
【學位授予單位】：重慶醫(yī)科大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TB33;TS255.7
本文編號：2461768
[Abstract]:Preservatives are usually used to keep vegetables fresh to prevent their decay. The majority of chemical preservatives are pesticides, which appear in the process of use, abuse, residue exceeding the standard and other phenomena, has seriously threatened the health of consumers. In the case of more and more attention to food safety, it is very important to find a safe and effective adsorbent for sample pretreatment. Magnetic nanomaterials (Fe_3O_4) are superparamagnetic and can be rapidly separated from the solution under the action of external magnetic field. By using the advantages of large specific surface area and low toxicity, and combining it with other materials, the extraction efficiency and separation speed can be improved. Graphene (G) is a two-dimensional crystal with only one layer of atom thickness formed by the hybridization of carbon atoms with sp2. It has a large specific surface area and a large conjugate system, which can withstand acid, alkali and heat resistance. Functionalized modification can be performed on the surface of G to produce different effects. Ionic liquid (IL) is composed of organic cations and inorganic or organic anions. Il is a liquid organic salt near room temperature. Il is widely used in organic synthesis and catalysis because of its excellent properties such as good thermal stability, strong solubility and so on. Separation analysis and other fields. In this paper, the preparation of new magnetic graphene complexes as purification adsorption materials to achieve rapid and effective detection of a variety of preservative in vegetables. The first part is based on the magnetic graphene composite rapid detection of 16 kinds of preservative in vegetables objective: based on the principle of Qu ECh ERS method, Fe_3O_4@Si O _ 2 / G composite material was prepared. It was used as an adsorbent for magnetic solid phase extraction of (MSPE) to purify vegetable samples rapidly. Sixteen preservative agents in vegetable samples were simultaneously determined by gas chromatography mass spectrometry (GC-MS). Methods: Fe_3O_4@Si O 2 / G was prepared by chemical bonding method. The ratio of synthesis was optimized. Vegetables were extracted with acetonitrile and cleaned up by Fe_3O_4@Si O 2? G, and quantified by external standard method of GC-MS. Results: the linear range of 16 preservatives was 0.02 ~ 2.00 mg/L, the correlation coefficient (R ~ 2) was 0.9946 渭 g / kg, the detection limit was 0.21 ~ 11.50 渭 g / kg, the recovery was 78.3% ~ 116.7%, the correlation coefficient was 0.9946 ~ 0.9998, the detection limit was 0.21 ~ 11.50 渭 g / kg, and the recovery was 78.3%. The relative standard deviation is 1.4% and 11.9%. Conclusion: the Fe_3O_4@Si O 2 G prepared in this paper has good adsorption ability and superparamagnetism, which greatly improves the separation speed. The detection results show that the method is rapid, accurate and sensitive. It can be applied to the determination of 16 kinds of preservative in actual vegetable samples. The second part is based on the rapid detection of 20 kinds of preservatives in vegetables based on magnetic graphene polyionic liquid composites. Objective: to prepare magnetic nanoparticles (Fe_3O_4) of 200 渭 1 000 nm. A rapid method for the determination of 20 preservative agents in vegetables was established by synthesizing Fe_3O_4@Si O2@G@PIL composites as adsorbents for improved Qu ECh ERS method combined with gas chromatography mass spectrometry (GC-MS). Methods: Fe_3O_4, composites with different particle sizes were prepared by chemical precipitation method, and then Fe_3O_4@Si O2@G@PIL composites with different particle sizes were prepared respectively. Using vegetables as raw materials and acetonitrile saturated with n-hexane, composite materials with different particle sizes were used as adsorbents for impurity removal. The effects were compared and quantified by GC-MS external standard method. Results: the calibration curves of 20 preservatives were linear at 0.02 ~ 2.00 mg/L, the correlation coefficient (R2) was 0.9972 渭 g / kg. and the detection limit was 0.82 ~ 6.64 渭 g / kg.. Conclusion: the prepared Fe_3O_4@Si O2@G@PIL composites have good adsorption properties and can be used for the rapid and efficient detection of 20 kinds of preservative in vegetable samples.
【學位授予單位】：重慶醫(yī)科大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TB33;TS255.7
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