摘要
目的利用在线捕集消除本底,同位素稀释技术,建立婴幼儿乳粉中双酚A和壬基酚的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。方法样品经乙腈超声提取,PSA/Silica固相萃取柱净化,超高效液相色谱-串联质谱进行测定,采用电喷雾电离负离子模式(ESI-),多反应监测(MRM),内标法定量分析。结果双酚A和壬基酚的浓度为0.40~100μg/L时,线性关系良好,相关系数(r)分别为0.999 6和0.999 2,方法的检出限为0.10μg/kg。双酚A和壬基酚在高中低加标浓度(50、10、2μg/L)的平均回收率分别为98.13%~103.67%、96.17%~105.58%,变异系数分别为4.23%~7.37%、5.14%~10.19%。结论该方法在样品处理过程中采用高温烘烤过的玻璃器皿,并利用在线捕集技术等降低本底,提高了检测的灵敏度,且定性定量准确,适用于婴幼儿乳粉中双酚A和壬基酚的检测。
Objective To establish a method with ultra-performance liquid chromatography tandem mass spectrometry （UPLC-MS/MS） to simultaneously detect bisphenol A and nonylphenol in infant milk powder with online capture and isotope dilution technologies. Methods The sample was extracted with acetonitrile,then the extract was cleaned up with PSA/Silica column. The reconstituted sample solution was analyzed using UPLC-MS/MS with multiple reaction mode （MRM） in negative ion,with an Acquity UPLC BEH C18 column（100 mm× 2.1 mm,1.7 μm） as the analytical column by internal standard method. Results The calibration curves were linear within the range of 0.40 μg/L-100μg/L, the correlation coefficient （ r ） was respectively 0. 999 6 and 0. 999 2. The limit of detection was 0.10 μg/kg. The method was validated at 50 μg/L, 10 μg/L, 2μg/L. The overall recoveries were 98. 13 %-103.67 % and 96.17 % 105.58 %, with the relative standard deviations of 4.23%-7.37%, and 5.14%-10.19%. Conclusion By using high temperature baked glassware and online capture technologies, the blank value can be reduced effectively, and the sensitivity is improved. The method is qualitative, quantitative and accurate, which is applicable to simultaneously determine bisphenol A and nonylphenol in infant milk powder.
出处
《预防医学论坛》
2017年第3期233-235,共3页
Preventive Medicine Tribune
关键词
超高效液相色谱-串联质谱法
婴幼儿乳粉
双酚A
壬基酚
Ultra-performance liquid chromatography tandem mass spectrometry （UPLC-MS/MS）
Infant milk powder
Bisphenol A
Nonylphenol
