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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0.5 mol/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0.13 mg/kg,定量限为0.42 mg/kg,加标回收率在90%~95%之间(添加水平分别为1、10、30 mg/kg),相对标准偏差小于5%.
Rapid determination of 4-aminoazobenzene released from azo dyes in food wrappers by high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) Specimens were prepared in a 0.5 mol / L sodium hydroxide solution , With sodium dithionite reduction of the sample of azo dyes, with methyl tert-butyl ether stripping reduction generated 4-amino-azobenzene, nitrogen blowing, methanol reconstituted, using liquid chromatography - tandem mass spectrometry The method was optimized by internal standard method.METHODS The conditions of chromatographic separation, mass spectrometry, liquid-liquid extraction and dispersive solid-phase extraction were optimized.The detection limit was 0.13 mg / kg, the limit of quantification was 0.42 mg / kg under the optimal conditions, The spiked recoveries ranged from 90% to 95% (1, 10 and 30 mg / kg, respectively), and the relative standard deviations were less than 5%.