毛細管區帶電泳分離檢測鷹爪蝦和紅頭魚中溴酚   全文下載

Separation and Determination of Bromophenols in Trachypenaeus curvirostris and Lepidotrigla microptera by Capillary Zone Electrophoresis

溴酚是動物源海洋食品的重要的風味化合物。本研究利用毛細管區帶電泳同時測定了動物源海洋食品中的4-溴苯酚、2,4,6-三溴酚、2,4-二溴酚、2-溴酚和2,6-二溴酚。最佳緩衝體係為20 mmol/L硼砂-NaOH緩衝液（pH值10.00），電壓為30 kV和280 nm紫外檢測。回歸方程顯示的線性關係良好（5種溴酚相關係數分別為：0.9990，0.9998，0.9997，0.9999和0.9995）。 4-溴苯酚、2,4,6-三溴酚、2,4-二溴酚、2-溴酚和2,6-二溴酚的線性範圍分別是：18.8 - 1200 μg/mL 、15 - 960 μg/mL 、9.4 - 600 μg/mL 、10.6 - 680 μg/mL 、11.6 - 740 μg/mL。同一天內遷移時間和峰面積的相對標準偏差分別小於2.1%和4.9%。回收率為91.5% - 103.4%。 4-溴苯酚、2,4,6-三溴酚、2,4-二溴酚、2 μ-溴酚和2,6-二溴酚的檢測線分別為1.6、1.9、1.2、0.9和1.4 g/mL。系統優化了影響分離的各種電泳參數。利用該方法對鷹爪蝦和紅頭魚中的溴酚化合物進行了測定，鷹爪蝦中4-溴苯酚、2,4,6-三溴酚、 2,4-二溴酚和2,6-二溴酚的含量分別是3.9、2.5、7.3和0.6 ng/g，而在淡水食品青蝦和鯽魚中均未發現溴酚類化合物。"

Bromophenols have been identified as key off-flavor compounds found in seafood. In this report, a new method of capillary zone electrophoresis (CZE) was established for simultaneous assay of five bromophenols, 4-bromophenol (4-BP), 2,4,6-tribromophenol (2,4,6-TBP), 2,4-dibromophenol (2,4-DBP), 2-bromophenol (2-BP) and 2,6-dibromophenol (2,6-DBP), in seafood. The optimum buffer system was 20 mM borate-NaOH buffer (pH 10.00). Voltage was +30 kV and the ultraviolet absorbance detection at 280 nm. The column was an uncoated 50 µm ID fused-silica capillary. Regression equations revealed linear relationships (correlation coefficients: 0.9990, 0.9998, 0.9997, 0.9999 and 0.9989) between the peak area of each compound and its concentration. Calibration curves were constructed in the range of 18.8 - 1200, 15 - 960, 9.4 - 600, 10.6 - 680 and 3.0 - 370 mg/mL for 4-BP, 2,4,6-TBP, 2,4-DBP, 2-BP and 2,6-DBP, respectively. The relative standard deviations of migration times and peak areas were < 2.1% and 4.9% within one day, respectively. The recoveries of bromophenols were 91.5 - 103.4%. The detection limits (S/N = 3) of 4-BP, 2,4,6-TBP, 2,4-DBP, 2-BP and 2,6-DBP were 1.6, 1.9, 1.2, 0.9 and 1.4 mg/mL, respectively. The effects of several CE parameters on the resolution were studied systematically. Compared with liquid chromatography, the method described here is relatively rapid and can give symmetrical peaks. The contents of 5 bromophenols in seafood (Trachypenaeus curvirostris and Lepidotrigla microptera) were determined with satisfactory repeatability and recovery. The contents of 4-BP, 2,4,6-TBP, 2,4-DBP and 2,6-DBP in T. curvirostris were 3.9, 2.5, 7.3 and 0.6 ng/g, respectively. The feasibility of this method for the determination of bromophenols in freshwater fish and crustaceans (Macrobrachium nipponense and Carassius auratus var. Pengzesis) also tested. The result indicated that these flavor compounds in freshwater fish and crustaceans were lower than the detection limits mentioned above.