乳制品中双酚类物质及其环氧衍生物的检测方法研究

发布时间：2018-07-22 16:39

【摘要】：双酚类物质及其环氧衍生物作为一类常见的内分泌干扰物,可通过包装材料接触等方式迁移到食品中。乳制品中双酚类及其环氧衍生物的检测具有重要意义。本论文对乳制品中该类物质的前处理和检测方法进行了研究探讨。对目标物进行乙酰化衍生,同时采用分散液液微萃取,发展了乳制品中双酚A和双酚F的气相色谱-串联质谱的检测方法。通过考察衍生条件和萃取条件,优化了前处理过程;通过优化质谱参数,提高了仪器灵敏度和选择性。最终,目标物在1～100 μg/L范围内线性关系良好,定量限为0.2～0.5 μg/kg,平均回收率在73.7%～84.2%之间,日内和日间精密度分别为3.0%～5.9%和3.9%～7.7%。采用固相萃取净化,结合高效液相色谱-荧光检测器,发展了乳制品中15种双酚类物质及其环氧衍生物的分析方法。通过考察色谱柱、流动相和柱温,优化了分离条件,同时筛选了提取溶剂、固相萃取柱、淋洗液及洗脱液,优化了前处理条件。方法学验证结果显示,15种目标物在其相应的浓度范围内线性关系良好,定量限为10～100 μg/kg,平均回收率范围为81.5%～97.5%。基于QuEChERS方法,结合超高效液相色谱-串联质谱,发展了乳制品中21种双酚类物质及其环氧衍生物的高通量筛查方法。通过对色谱质谱参数及前处理条件的优化,最终建立了简单、快速、灵敏的分析方法。各目标物在其相应的浓度范围内线性关系良好(r20.991),定量限为0.02～50.00 μg/kg,平均回收率在88.2%～108.2%之间。
[Abstract]:Bisphenols and their epoxy derivatives, as a common endocrine disruptor, can be transferred to food by contact with packaging materials. The detection of bisphenol and its epoxy derivatives in dairy products is of great significance. In this paper, the pretreatment and detection methods of this kind of substances in dairy products were studied. The determination method of bisphenol A and bisphenol F in dairy products by gas chromatography-tandem mass spectrometry (GC-MS) was developed. The pretreatment process was optimized by investigating the derivation conditions and extraction conditions, and the sensitivity and selectivity of the instrument were improved by optimizing the parameters of mass spectrometry. In the end, the linear range of the target is 1 ~ 100 渭 g / L, the quantitative limit is 0.2 ~ 0.5 渭 g / kg, the average recovery is between 73.7% and 84.2%, the intra-day and inter-day precision are 3.0% and 5.9% and 3.9 渭 g 路kg ~ (-1), respectively. A method for the determination of 15 bisphenols and their epoxide derivatives in dairy products was developed by solid phase extraction (SPE) and high performance liquid chromatography (HPLC)-fluorescence detector. The separation conditions were optimized by investigating the chromatographic column, mobile phase and column temperature. At the same time, the extraction solvent, solid phase extraction column, elution solution and elution solution were screened, and the pretreatment conditions were optimized. The results of methodology verification showed that there was a good linear relationship between the 15 target compounds in the corresponding concentration range, the quantitative limit was 10 ~ 100 渭 g / kg, and the average recovery range was 81.5 ~ 97.5 渭 g 路kg ~ (-1) 路L ~ (-1) ~ (-1) ~ (-1). Based on QuEChERS method and ultrahigh performance liquid chromatography-tandem mass spectrometry, a high-throughput screening method for 21 bisphenols and their epoxide derivatives in dairy products was developed. A simple, rapid and sensitive analytical method was established by optimizing the parameters of chromatography-mass spectrometry and pretreatment conditions. The linear range of each target was good (r 20.991), the limit of quantification was 0.02n 50.00 渭 g / kg, and the average recovery was between 88.2% and 108.2%.
【学位授予单位】：华东理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TS252.7

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