分散液液微萃
發(fā)布時間：2018-12-20 21:20
【摘要】：食品中農(nóng)藥殘留的積累嚴重影響了人類的身心健康,建立簡單有效的檢測方法至關(guān)重要。分散液液微萃取是一種新型的前處理方式,具有有機溶劑用量少、操作簡單、富集倍數(shù)高、靈敏度高等優(yōu)點,本文采用分散液液微萃取的前處理方式結(jié)合氣質(zhì)聯(lián)用、液質(zhì)聯(lián)用的多反應(yīng)監(jiān)測模式,檢測食品中酰胺類除草劑、有機磷及新型殺蟲劑的殘留,有效地降低了基質(zhì)的影響。主要的研究內(nèi)容及結(jié)果如下:1.采用鹽析-渦旋輔助分散液液微萃取-氣質(zhì)聯(lián)用快速測定食品中的8種酰胺類除草劑的殘留,多反應(yīng)監(jiān)測模式,外標法定量分析。探究分散液液微萃取-氣相色譜-質(zhì)譜的最佳條件,對萃取劑和分散劑的種類、體積,渦旋時間、離子強度及離心時間進行了優(yōu)化。最佳條件:分散劑為9.5 m L乙腈,萃取劑為30μL溴苯,渦旋5 s,4000 r/min離心6 min。8種酰胺類農(nóng)藥的檢出限范圍為0.03~0.6 ng/L,定量限為1.0ng/L,相關(guān)系數(shù)0.992,富集倍數(shù)為3480~3920,日內(nèi)、日間相對標準偏差9.6%,加標250 ng/L、750 ng/L,樣品回收率為87~103%,萃取效率高,方法重復(fù)性好,適合蔬菜茶葉等農(nóng)藥殘留分析。2.采用鹽析-渦旋輔助分散液液微萃取-液質(zhì)聯(lián)用測定茶葉、果汁中6種有機磷農(nóng)藥殘留,以甲醇-水為流動相(含0.1%甲酸),質(zhì)譜正離子多反應(yīng)監(jiān)測模式,外標法定量分析。實驗對分散液液微萃取方法中的萃取劑、分散劑的種類和體積,前后渦旋時間、離子強度等條件進行了優(yōu)化,最佳條件:7.5 mL正丙醇為分散劑,30μL 1-溴-3-甲基丁烷為萃取劑,離子強度加NaCl 0.5 g,前渦旋時間2 min,后渦旋時間為50 s。6種有機磷檢出限范圍是10~25 ng/L,定量限為50.0 ng/L,相關(guān)系數(shù)0.990,富集倍數(shù)約為3640~4120,日內(nèi)、日間相對標準偏差10.6%,加標200 ng/L、800 ng/L進行回收實驗,回收率為85~107%。是一種簡便、快速的農(nóng)藥多殘留分析方法。3.建立一種微固相萃取-分散液液微萃取-液質(zhì)聯(lián)用的檢測茶葉、果汁中4種殺蟲劑的農(nóng)藥殘留的分析方法,以乙腈-水為流動相(含0.1%甲酸),質(zhì)譜采用正離子多反應(yīng)監(jiān)測模式,外標法定量分析。采用金屬有機骨架納米材料做固相萃取吸附劑,減少了基質(zhì)的影響,極大程度上提高了靈敏度。實驗主要從納米材料的種類、用量、萃取劑和分散劑的種類和用量、渦旋時間等方面優(yōu)化實驗條件,最佳條件:150 mg MIL-100(Fe),乙腈為洗脫劑和分散劑,1.3 mL/次,洗脫3次,40μL溴苯為萃取劑,渦旋時間50 s,4種合成類殺蟲劑檢出限范圍是0.3~0.6 ng/L,定量限為1.0 ng/L,相關(guān)系數(shù)0.993,富集倍數(shù)約為890~990,日內(nèi)、日間相對標準偏差9.3%,加標250 ng/L、750 ng/L進行回收實驗,回收率為88~103%。該方法有機溶劑用量少,基質(zhì)影響小,富集倍數(shù)和靈敏度高,適用于食品中較復(fù)雜基質(zhì)的農(nóng)藥殘留檢測。
[Abstract]:The accumulation of pesticide residues in food seriously affects the physical and mental health of human beings. It is very important to establish a simple and effective method for the determination of pesticide residues. Dispersion liquid microextraction is a new pretreatment method, which has the advantages of less organic solvent consumption, simple operation, high enrichment factor, high sensitivity and so on. In this paper, dispersion liquid microextraction is combined with GC-MS. The multi-reaction monitoring model with liquid-mass spectrometry was used to detect the residues of herbicides, organophosphorus and new insecticides in food, which effectively reduced the effect of substrate. The main contents and results are as follows: 1. The residues of 8 kinds of amide herbicides in food were determined rapidly by salting-vortex assisted dispersible liquid microextraction and GC-MS. The multi-reaction monitoring model and external standard method were used for quantitative analysis. The optimum conditions of dispersible liquid-liquid microextraction-gas chromatography-mass spectrometry (GC-MS) were investigated, and the types, volume, vortex time, ionic strength and centrifugal time of extractant and dispersant were optimized. The optimum conditions were as follows: dispersant was 9.5 mL acetonitrile, extraction agent was 30 渭 L bromobenzene, vortex 5 s-1 4 000 r/min centrifugation 6 min.8 amides, the detection limit was 0.03? 0. 6 ng/L, quantitative limit was 1.0 ng / L. The correlation coefficient was 0.992, the enrichment multiple was 3480 ~ 3920, the relative standard deviation was 9.6, the recovery rate of the sample was 87 ~ 103, the extraction efficiency was high, and the method was reproducible. Suitable for pesticide residue analysis of vegetables, tea, etc. 2. Six organophosphorus pesticide residues in tea juice were determined by salting-vortex assisted dispersive liquid microextraction and liquid-mass spectrometry. The mobile phase of methanol-water (containing 0.1% formic acid) was used. Quantitative analysis of external standard method. The extractant, the type and volume of dispersant, the vortex time and ionic strength were optimized. The optimum conditions were as follows: 7.5 mL n-propanol was used as dispersant. 30 渭 L 1-bromo-3-methylbutane was used as extractant, ion strength and NaCl were 0.5 g, and the detection limit of 50 s. 6 organophosphorus was 50 s. 6 after 2 min,. The quantitative limit of 10 ~ 25 ng/L, was 50.0 ng/L,. The correlation coefficient was 0.990, and the enrichment multiple was about 3640 ~ 4120. Within days, the relative standard deviation between days was 10.6 and the recovery rate was 85 ~ 1070.The recovery rate was 85,1070.The correlation coefficient was 0.990 and the relative standard deviation was 10.6. It is a simple and rapid method for multiresidue analysis of pesticides. A method for the determination of pesticide residues in tea and juice by microsolid phase extraction-dispersion liquid microextraction and liquid-mass spectrometry was established. Acetonitrile-water was used as mobile phase (0.1% formic acid). The mass spectrometry adopts the positive ion multi-reaction monitoring mode, and the external standard method is used for quantitative analysis. Using organometallic nanomaterials as solid phase extraction adsorbent, the influence of matrix is reduced, and the sensitivity is greatly improved. The experimental conditions were optimized from the aspects of the kinds and amounts of nano-materials, the kinds and amounts of extractant and dispersant, the vortex time and so on. The optimum conditions were as follows: 150 mg MIL-100 (Fe), acetonitrile as eluent and dispersant, 1.3 mL/, etc. Three times elution, 40 渭 L bromobenzene as extractant, and the detection limit of 40 渭 L bromobenzene as extractant. The detection limit of 40 渭 L bromobenzene was 0. 3N 0. 6 ng/L,. The correlation coefficient was 0. 993, and the enrichment multiple was about 89. 990, within a day. The recovery experiment was carried out by adding standard 250 ng/L,750 ng/L, and the recovery rate was 88% 103.The relative standard deviation (RSDs) was 9.3% during the day. The method is suitable for the determination of pesticide residues in more complex matrix in food because of its small amount of organic solvent, little influence on matrix, high enrichment factor and high sensitivity.
【學位授予單位】：山西大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TS207.53;O657.63
本文編號：2388423
[Abstract]:The accumulation of pesticide residues in food seriously affects the physical and mental health of human beings. It is very important to establish a simple and effective method for the determination of pesticide residues. Dispersion liquid microextraction is a new pretreatment method, which has the advantages of less organic solvent consumption, simple operation, high enrichment factor, high sensitivity and so on. In this paper, dispersion liquid microextraction is combined with GC-MS. The multi-reaction monitoring model with liquid-mass spectrometry was used to detect the residues of herbicides, organophosphorus and new insecticides in food, which effectively reduced the effect of substrate. The main contents and results are as follows: 1. The residues of 8 kinds of amide herbicides in food were determined rapidly by salting-vortex assisted dispersible liquid microextraction and GC-MS. The multi-reaction monitoring model and external standard method were used for quantitative analysis. The optimum conditions of dispersible liquid-liquid microextraction-gas chromatography-mass spectrometry (GC-MS) were investigated, and the types, volume, vortex time, ionic strength and centrifugal time of extractant and dispersant were optimized. The optimum conditions were as follows: dispersant was 9.5 mL acetonitrile, extraction agent was 30 渭 L bromobenzene, vortex 5 s-1 4 000 r/min centrifugation 6 min.8 amides, the detection limit was 0.03? 0. 6 ng/L, quantitative limit was 1.0 ng / L. The correlation coefficient was 0.992, the enrichment multiple was 3480 ~ 3920, the relative standard deviation was 9.6, the recovery rate of the sample was 87 ~ 103, the extraction efficiency was high, and the method was reproducible. Suitable for pesticide residue analysis of vegetables, tea, etc. 2. Six organophosphorus pesticide residues in tea juice were determined by salting-vortex assisted dispersive liquid microextraction and liquid-mass spectrometry. The mobile phase of methanol-water (containing 0.1% formic acid) was used. Quantitative analysis of external standard method. The extractant, the type and volume of dispersant, the vortex time and ionic strength were optimized. The optimum conditions were as follows: 7.5 mL n-propanol was used as dispersant. 30 渭 L 1-bromo-3-methylbutane was used as extractant, ion strength and NaCl were 0.5 g, and the detection limit of 50 s. 6 organophosphorus was 50 s. 6 after 2 min,. The quantitative limit of 10 ~ 25 ng/L, was 50.0 ng/L,. The correlation coefficient was 0.990, and the enrichment multiple was about 3640 ~ 4120. Within days, the relative standard deviation between days was 10.6 and the recovery rate was 85 ~ 1070.The recovery rate was 85,1070.The correlation coefficient was 0.990 and the relative standard deviation was 10.6. It is a simple and rapid method for multiresidue analysis of pesticides. A method for the determination of pesticide residues in tea and juice by microsolid phase extraction-dispersion liquid microextraction and liquid-mass spectrometry was established. Acetonitrile-water was used as mobile phase (0.1% formic acid). The mass spectrometry adopts the positive ion multi-reaction monitoring mode, and the external standard method is used for quantitative analysis. Using organometallic nanomaterials as solid phase extraction adsorbent, the influence of matrix is reduced, and the sensitivity is greatly improved. The experimental conditions were optimized from the aspects of the kinds and amounts of nano-materials, the kinds and amounts of extractant and dispersant, the vortex time and so on. The optimum conditions were as follows: 150 mg MIL-100 (Fe), acetonitrile as eluent and dispersant, 1.3 mL/, etc. Three times elution, 40 渭 L bromobenzene as extractant, and the detection limit of 40 渭 L bromobenzene as extractant. The detection limit of 40 渭 L bromobenzene was 0. 3N 0. 6 ng/L,. The correlation coefficient was 0. 993, and the enrichment multiple was about 89. 990, within a day. The recovery experiment was carried out by adding standard 250 ng/L,750 ng/L, and the recovery rate was 88% 103.The relative standard deviation (RSDs) was 9.3% during the day. The method is suitable for the determination of pesticide residues in more complex matrix in food because of its small amount of organic solvent, little influence on matrix, high enrichment factor and high sensitivity.
【學位授予單位】：山西大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TS207.53;O657.63
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，本文編號：2388423
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