【摘要】：雙酚類物質(zhì)及其環(huán)氧衍生物作為一類常見的內(nèi)分泌干擾物,可通過包裝材料接觸等方式遷移到食品中。乳制品中雙酚類及其環(huán)氧衍生物的檢測具有重要意義。本論文對(duì)乳制品中該類物質(zhì)的前處理和檢測方法進(jìn)行了研究探討。對(duì)目標(biāo)物進(jìn)行乙�；苌�,同時(shí)采用分散液液微萃取,發(fā)展了乳制品中雙酚A和雙酚F的氣相色譜-串聯(lián)質(zhì)譜的檢測方法。通過考察衍生條件和萃取條件,優(yōu)化了前處理過程;通過優(yōu)化質(zhì)譜參數(shù),提高了儀器靈敏度和選擇性。最終,目標(biāo)物在1～100 μg/L范圍內(nèi)線性關(guān)系良好,定量限為0.2～0.5 μg/kg,平均回收率在73.7%～84.2%之間,日內(nèi)和日間精密度分別為3.0%～5.9%和3.9%～7.7%。采用固相萃取凈化,結(jié)合高效液相色譜-熒光檢測器,發(fā)展了乳制品中15種雙酚類物質(zhì)及其環(huán)氧衍生物的分析方法。通過考察色譜柱、流動(dòng)相和柱溫,優(yōu)化了分離條件,同時(shí)篩選了提取溶劑、固相萃取柱、淋洗液及洗脫液,優(yōu)化了前處理?xiàng)l件。方法學(xué)驗(yàn)證結(jié)果顯示,15種目標(biāo)物在其相應(yīng)的濃度范圍內(nèi)線性關(guān)系良好,定量限為10～100 μg/kg,平均回收率范圍為81.5%～97.5%�；赒uEChERS方法,結(jié)合超高效液相色譜-串聯(lián)質(zhì)譜,發(fā)展了乳制品中21種雙酚類物質(zhì)及其環(huán)氧衍生物的高通量篩查方法。通過對(duì)色譜質(zhì)譜參數(shù)及前處理?xiàng)l件的優(yōu)化,最終建立了簡單、快速、靈敏的分析方法。各目標(biāo)物在其相應(yīng)的濃度范圍內(nèi)線性關(guān)系良好(r20.991),定量限為0.02～50.00 μg/kg,平均回收率在88.2%～108.2%之間。
[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%.
【學(xué)位授予單位】：華東理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TS252.7

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