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

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。

Synchronous Fluorescence Determination of Tryptamine in Soy Sauce Using Three phase Hollow Fiber Liquid Phase Microextraction Coupled with Thin-layer Chromatography

A novel method of hollow fiber liquid phase microextraction (HF-LPME) coupled with thin-layer chromatography was developed for the synchronous spectrofluorimetric determination of tryptamine in soy sauce.The optimum extraction was achieved by adjusting pH value of sample solution to 12.0,using 1-octanol as organic extraction solvent,and 0.1 mol/L HCl as the acceptor phase,and stirring the solution at 590 r/min for 60 min.After extraction,20 μL portion of accepter phase was applied for TLC separation,and the analyte spot was washed off with isopropanol.The quantification analysis of tryptamine was performed with synchronous fluorescence spectra at 350.4 nm.Under the optimum conditions,the calibration curve showed a good linearity in the range of 0.32-50 mg/L(r ＞0.978 0).The detection limit was 0.32 mg/L.The spiked recoveries from soy sauce samples were in the range of 87.5％-107.7％ with RSDs not more than 6.6％.The proposed method was simple,sensitive,green and accurate,and was suitable for the determination of tryptamine in soy sauce.