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本研究建立了快速基质分散固相萃取(quick easy cheap effective rugged and safe,Qu ECh ERS)—固相萃取(Solid phase extraction,SPE)样品净化,液相色谱三重四级杆串联质谱测定婴幼儿配方奶中八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,Qu ECh ERS-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八种双酚类化合物的基质因子为0.80~1.03;在线性范围内,八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每日可能最多摄入BPA、BPF、BPS量分别为0.065、0.050、0.0059μg/kg bw(body weight)/day,但均未超过欧洲食品安全协会对双酚类物质从食品包装材料迁移到食品中限量的规定(4μg/kg bw/day)。
In this study, QuECh ERS and SPE were used to purify the sample. The liquid chromatography triple quadrupole mass spectrometry was used to determine the formula of infant formula Method for the Residues of Eight Bisphenols in Milk. Residues of the bisphenols in the samples were extracted with acetonitrile and Qu ECh ERS-SPE was used to clean the samples. The matrix matching standard was calibrated by external standard method. The results showed that the matrix factors of the eight bisphenols purified and calibrated were 0.80 ~ 1.03. The linear correlation coefficients (R2) of eight bisphenols were all greater than 0.999 in the linear range. The method recoveries ranged from 50.2% to 116% (n = 6) with relative standard deviations of 0.5% to 14% (n = 6). The detection limits and the limits of quantitation were 0.017-0.78μg / kg for solid milk powder and 0.055 ~ 2.6μg / kg, liquid milk was 0.0011 ~ 0.055μg / L and 0.0035 ~ 0.18μg / L. This method is used to test the infant formula purchased in China and Canada. Based on the measured content and the daily intake of milk, the daily maximum intake of BPA may be calculated respectively. The quantities of BPF and BPS are respectively 0.065, 0.050 and 0.0059 μg / kg bw body weight / day respectively, all of which did not exceed the requirements of the European Food Safety Association (4 μg / kg bw / day) for the migration of bisphenols from food packaging materials to food products.