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目的建立在线捕集消除本底-超高效液相色谱-串联质谱法测定婴幼儿辅助食品中双酚A和壬基酚的方法。方法样品经环己烷-乙酸乙酯超声提取,凝胶色谱(GPC)除酯净化,超高效液相色谱-串联质谱法测定,内标法定量。并对双酚A和壬基酚测定中存在的本底及消除方法进行了研究。结果双酚A和壬基酚的浓度为0.5μg/L~150μg/L时,线性关系良好,相关系数(r)分别为0.999 5和0.999 3,方法的检出限为0.1μg/kg。在加标水平为0.5μg/kg、1.0μg/kg、10.0μg/kg时,样品中2种待测物的平均加标回收率为97.0%~116.0%,相对标准偏差(RSD)为6.4%~17.0%。结论在样本处理过程中选用高温烘烤过的玻璃器皿和没有本底的试剂;在仪器测定过程中换用管路,并辅以在线捕集技术消除流动相本底,有效降低了空白值,提高了灵敏度。该方法灵敏度高,定性、定量准确,非常适合婴幼儿辅助食品中双酚A和壬基酚的测定。
OBJECTIVE To establish a method for online determination of bisphenol A and nonylphenol in infant supplementary food by ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with cyclohexane - ethyl acetate, gel purified by GPC, and determined by ultra performance liquid chromatography - tandem mass spectrometry. The background and elimination methods of the determination of bisphenol A and nonylphenol were studied. Results When the concentrations of bisphenol A and nonylphenol were 0.5μg / L ~ 150μg / L, the correlation coefficients (r) were 0.999 5 and 0.999 3, respectively. The detection limit was 0.1 μg / kg. The spiked recoveries of two analytes in samples were 97.0% ~ 116.0% and the relative standard deviations (RSDs) were 6.4% at the spiked levels of 0.5μg / kg, 1.0μg / kg and 10.0μg / ~ 17.0%. Conclusion In the process of sample selection, the glassware baked at high temperature and the reagent without background were selected. The pipeline was replaced during the process of instrument determination, and the on-line trapping technique was used to eliminate the mobile phase background, effectively reducing the blank value and increasing Sensitivity The method has high sensitivity, qualitative and quantitative accuracy, and is very suitable for the determination of bisphenol A and nonylphenol in infant auxiliary food.