中空纤维三相液相微萃取-薄层色谱分离同步荧光法测定酱油中的色胺含量

发布时间：2019-06-20 17:17

【摘要】：以三相中空纤维液相微萃取(HF-LPME)作为样品前处理方法,结合薄层色谱分离,同步荧光光谱法测定酱油中色胺的含量。通过单因素实验确立的萃取最优条件为:样品溶液p H值为12.0,正辛醇为萃取溶剂,0.1 mol/L的HCl为接受相,搅拌速度为590 r/min,萃取时间为60 min;取20μL接受相进行TLC分析,样品点用异丙醇溶解后离心分离;采用同步荧光在λem=350.4 nm处进行定量分析。在最佳萃取条件下,方法的线性范围为0.32~50 mg/L(r0.978 0),检出限(S/N=3)为0.32 mg/L。酱油样品的加标回收率为87.5%~107.7%,相对标准偏差(RSD)不大于6.6%。该方法操作简单、绿色高效、灵敏度高,可用于酱油中色胺的快速准确测定。
[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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