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中空纖維三相液相微萃取-薄層色譜分離同步熒光法測定醬油中的色胺含量

發(fā)布時間:2019-06-20 17:17
【摘要】:以三相中空纖維液相微萃取(HF-LPME)作為樣品前處理方法,結(jié)合薄層色譜分離,同步熒光光譜法測定醬油中色胺的含量。通過單因素實驗確立的萃取最優(yōu)條件為:樣品溶液p H值為12.0,正辛醇為萃取溶劑,0.1 mol/L的HCl為接受相,攪拌速度為590 r/min,萃取時間為60 min;取20μL接受相進行TLC分析,樣品點用異丙醇溶解后離心分離;采用同步熒光在λem=350.4 nm處進行定量分析。在最佳萃取條件下,方法的線性范圍為0.32~50 mg/L(r0.978 0),檢出限(S/N=3)為0.32 mg/L。醬油樣品的加標(biāo)回收率為87.5%~107.7%,相對標(biāo)準(zhǔn)偏差(RSD)不大于6.6%。該方法操作簡單、綠色高效、靈敏度高,可用于醬油中色胺的快速準(zhǔn)確測定。
[Abstract]:The content of tryptamine in soy sauce was determined by synchronous fluorescence spectrometry with three-phase hollow fiber liquid phase microextraction (HF-LPME) as sample pretreatment method combined with thin layer chromatography. The optimum extraction conditions established by single factor experiment are as follows: the pH value of the sample solution is 12.0, the n-octanol is the extraction solvent, the HCl of 0.1 mol/L is the receiving phase, the stirring speed is 590 r 路min, the extraction time is 60 min;, the 20 渭 L receiving phase is taken for TLC analysis, the sample points are dissolved with isopropanol and separated by centrifugation, and the quantitative analysis is carried out at 位 em=350.4 nm by synchronous fluorescence. Under the optimum extraction conditions, the linear range of the method is 0.32 鈮,

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