QuEChERS-SPE快速样品制备-超高效液相色谱-串联质谱联用法测定婴幼儿配方奶中双酚类化合物

建立QuEChERS-固相萃取（quick, easy, cheap, effective, rugged, safe-solid phase extraction，QuEChERS-SPE）样品净化，超高效液相色谱-串联质谱测定婴幼儿配方奶中8 种双酚类化合物残留的方法。样品中的双酚类化合物残留经乙腈提取，QuEChERS-SPE净化样品，基质匹配标准校正外标法定量。结果表明，样品经净化和校正后8 种双酚类化合物的基质因子为0.80～1.20；在线性范围内，8 种双酚类化合物线性相关系数（R2）均大于0.999。方法回收率为50.2%～116%（n=6），相对标准偏差为0.5%～14%（n=6），方法的检出限和定量限：固体奶粉为0.017～0.78μg/kg及0.055～2.6μg/kg，液体奶为0.0011～0.055μg/L及0.0035～0.18μg/L。采用本方法对中国和加拿大市场购买的婴幼儿配方奶进行检测，根据测定的含量和婴幼儿每天摄入奶量，可分别计算出婴幼儿可能最多摄入双酚A、双酚S、双酚F的量分别为0.065、0.050、0.0059μg/（kg·d），但均未超过欧洲食品安全协会对双酚类化合物从食品包装材料迁移到食品中限量的规定（4μg/（kg·d））。

Determination of Bisphenol Compounds in Infant Formula by QuEChERS-SPE Rapid Sample Preparation and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A robust analytical method was established for the determination of eight bisphenol compounds in infant formula by using quick, easy, cheap, effective, rugged, safe-solid phase extraction (QuEChERS-SPE) for sample preparation and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for compound identification and quantitation. Bisphenol compounds from samples were extracted with acetonitrile, and the extract was subjected to sequential QuEChERS-SPE treatment to remove background interferences. The matrix-matched standard calibration method was used for quantitation. The results showed great reduction of the matrix effect with corrected matrix factor ranging 0.80–1.20 for the 8 bisphenols. within the linear range, the correlation coefficients (R2) of the calibration curves for the compounds were greater than 0.999. The method recovery was 50.2%?116% (n = 6) with relative standard deviations of 0.5%?14%. The limits of detection (LODs) and the limits of quantification (LOQs) were 0.017?0.78 and 0.055?2.6 μg/kg for milk powder, and 0.001 1?0.055 and 0.003 5?0.18 μg/L for liquid milk, respectively. The method was applied to different brands of infant formulas in Chinese and Canadian markets. Based on measured concentrations and infant daily consumption of milk, the potential dietary intakes of BPA, BPF and BPS (calculated from the highest concentrations) were estimated to be 0.065, 0.050, and 0.005 9 μg/(kg·d), respectively. The estimated intakes did not exceed the tolerable daily intake (4 μg/(kg·d)) set by the European Food Safety Association.