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建立了快速检测金枪鱼罐头中BPA、BADGE、BFDGE及其衍生物10种环境激素含量的超高效液相色谱-串联质谱法。样品经C18色谱柱分离,以乙酸铵溶液和甲醇为流动相梯度洗脱,质谱多反应监测(MRM)模式检测,基质标准校正,外标法定量。结果表明,BPA、BADGE·2HCl及其他环境激素分别在0.5~100μg/L,0.5~50μg/L和0.1~0μg/L范围内线性关系良好;定量限(以信噪比≥10计)为0.5μg/kg(BADGE·2HCl为1μg/kg);在3个加标水平下10种环境激素的加标回收率为71.32%~96.14%,相对标准偏差为3.19%~6.79%(n=6)。该方法具有优异的灵敏度与稳定性,满足对金枪鱼罐头中BPA,BADGE、BFDGE及其衍生物的痕量分析检测及准确定量。
A rapid ultra performance liquid chromatography-tandem mass spectrometry (tandem mass spectrometry) method was developed for rapid determination of 10 environmental hormones including BPA, BADGE, BFDGE and their derivatives in tuna cans. Samples were separated on a C18 column, eluted with a gradient of ammonium acetate and methanol, and detected by MRM (multi-reaction monitoring), matrix calibration and external standard method. The results showed that the linear relationship between BPA, BADGE · 2HCl and other environmental hormones in the range of 0.5 ~ 100μg / L, 0.5 ~ 50μg / L and 0.1 ~ 0μg / L were good. The limit of quantification μg / kg (1μg / kg for BADGE · 2HCl). The spike recoveries of 10 environmental hormones were 71.32% ~ 96.14% with relative standard deviations of 3.19% ~ 6.79% . The method has excellent sensitivity and stability to meet the detection and accurate quantification of trace analysis of BPA, BADGE, BFDGE and their derivatives in tuna cans.