E-alert液液萃取结合分散固相萃取-液相色谱串联质谱检测食品包装纸中的4-氨基偶氮苯
Determination of 4-Aminoazobenzene in Paper Packaging by Liquid Chromatography Tandem Mass Spectrometry Combining with Liquid-Liquid Extraction and Dispersive Solid-Phase Extraction
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摘要: 采用高效液相色谱-串联质谱法(LC-MS/MS)快速测定食品包装纸中偶氮染料释放的4-氨基偶氮苯.试样在0.5mol/L氢氧化钠溶液的碱性环境下, 用连二亚硫酸钠还原试样中的偶氮染料, 用甲基叔丁基醚反萃取还原裂解产生的4-氨基偶氮苯, 经氮吹、甲醇复溶后, 用液相色谱-串联质谱进行测定, 内标法定量.方法优化了色谱分离、质谱、液液萃取和分散固相萃取等条件.最优化条件下方法的检出限为0.13mg/kg, 定量限为0.42mg/kg, 加标回收率在90%~95%之间(添加水平分别为1、10、30mg/kg), 相对标准偏差小于5%.Abstract: A liquid chromatography-tandem mass spectrometric(LC-MS/MS), method for the quick detection of 4-Aminoazobenzene released from azo dyes in food wrappers, has been established. Sodium dithionite was added to sodium hydroxide solution to reduce and decompose the possible azo dyes. The extract was analyzed by liquid chromatography with tandem mass chromatography for the quantification and confirmation after a liquid-liquid extraction and dispersive solid-phase extraction. The chromatographic separations were performed on a ZORBAX Eclipse XDB-C18 column with gradient elution. In this method the conditions of chromatographic separation, mass spectrum, liquid-liquid extraction and dispersive solid-phase extraction were optimized. The detection limit was 0.13 mg/kg and the quantification limit was 0.42 mg/kg under optimal conditions, the spiking standard recoveries were ranged from 90%~95% with relative standard deviations (RSDs)≤5%.
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