UPLC-MS/MS测定婴幼儿配方乳粉中双酚A和壬基酚

建立一种测定婴幼儿配方乳粉中双酚A和壬基酚的超高效液相色谱串联质谱准确定性定量方法。向配方乳粉样品中加水溶解,乙腈提取,使用在线捕集技术消除流动相中的本底影响,以甲醇-0.1%氨水溶液作为流动相在C₁₈色谱柱上进行梯度洗脱,用超高效液相色谱仪进行分离后,通过电喷雾负离子模式电离,多反应检测模式进行检测分析,内标法准确定量。结果表明:在1~2000 ng/mL范围内呈良好的线性关系,相关系数大于0.999。本方法BPA和NP检出限均低至0.1 μg/kg,在不同婴幼儿配方乳粉中添加1、10、100 μg/kg三水平加标,测定结果平均回收率在89.5%~102.8%之间,相对标准偏差为1.3%~4.8%,该方法具有较高的灵敏度和准确度。对市售200份婴幼儿配方乳粉进行测定,检出BPA含量为0.1~30.0 μg/kg,检出NP含量为1.1~105 μg/kg,适合婴幼儿配方乳粉中双酚A和壬基酚的定量测定。

Determination of Bisphenol A and Nonylphenol in Infant Formula Milk Powder by UPLC-MS/MS

An accurate qualitative and quantitative method was established for determination of bisphenol A and nonylphenol in infant formula milk powder by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Infant formula milk powder was dissolved in water,extracted by acetonitrile,online capture technology can eliminate background effects in mobile phase. Gradient elution was carried out on C₁₈ column with methanol-0.1% ammonia solution as mobile phase,then the identification and quantitation of bisphenol A and nonylphenol was performed by MS/MS in negative electrospray ionization(ESI-)and multiple reaction monitoring(MRM)mode. The results showed that there was a good linear relationship in the range of 1~2000 ng/mL. The correlation coefficient was greater than 0.999.The detection limits of BPA and NP in this method were 0.1 μg/kg. Three levels of 1,10 and 100 μg/kg were added to different infant formula milk powder. The average recovery of the results was 89.5%~102.8%,and the relative standard deviation was from 1.3% to 4.8%. The method had high sensitivity and accuracy. 200 samples of infant formula milk powder purchased from the market were determined. bisphenol A content was 0.1~30.0 μg/kg and nonylphenol content was 1.1~105 μg/kg,which was suitable for quantitative determination of bisphenol A and nonylphenol in infant formula milk powder.