固相萃取-超高效液相色谱-串联质谱法测定瓶装饮用水中双酚A、双酚S  

Determination of bisphenol A and bisphenol S residues in bottled drinking water by ultra performance liquid chromatography-tandem mass spectrometry with solid phase extraction

作　　者：张媛媛[1] 李延升[1] 韩晓鸥[1] 陈曦[1] 高岩[1] ZHANG Yuan-Yuan;LI Yan-Sheng;HAN Xiao-Ou;CHEN Xi;GAO Yan(Center for Disease Control and Prevention of Liaoning Province, Shengyang 110005, China)

机构地区：[1]辽宁省疾病预防控制中心,沈阳110005

出　　处：《食品安全质量检测学报》2018年第9期2158-2163,共6页Journal of Food Safety and Quality

摘　　要：目的建立固相萃取(solid phase extraction,SPE)结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定瓶装饮用水中双酚A(bisphenol A,BPA)、双酚S(bisphenol S,BPS)的方法。方法利用BPA-D_4和BPS-^(13)C_(12)混合同位素内标,经Waters Oasis系列的HLB固相萃取柱富集样品,以甲醇-水为流动相,经Waters BEH C_(18)色谱柱分离,采用UPLC-MS/MS在负离子电离(electron spray ionization,ESI-)模式和多反应监控(multiple reaction monitoring,MRM)模式下检测。结果用该方法测定时,BPA在1~50μg/L范围内线性良好,BPS在0.2~10μg/L范围内线性良好,相关系数r均为0.9999,BPA的平均回收率为99.5%~100.7%,相对标准偏差为0.8%~4.6%;BPS的平均回收率为95.9%~102.1%,相对标准偏差为1.3%~2.5%,BPA的最低检出浓度为20 ng/L,BPS的最低检出浓度为5 ng/L。结论此方法操作简单、灵敏度高、重现性好,适用于瓶装饮用水中双酚A、双酚S的检测。Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） with solid phase extraction （SPE） method for the determination ofbisphenol A （BPA） and bisphenol S （BPS） in bottled drinking water. Methods With BPA-D4 and BPS-13C12 isotope as mixed internal standards, the BPA and BPS were enriched by Waters Oasis HLB column. The samples were separated by Waters BEH C18 chromatographic column with methanol-water as mobile phase, and then detected by UPLC-MS/MS under the multiple reactions monitoring （MRM） mode with the negative-ion mode and quantified by an internal standard method. Results Using the established method, BPA and BPS had good linearities in the ranges of 1-50 μg/L and 0.2-10 μg/L for BPA and BPS, respectively （r〉0.999）. The average recoveries of BPA were 99.5%-100.7% and the relative standard deviations were 0.8%-4.6%. The average recoveries of BPS were 95.9%-102.1% and the relative standard deviations were 1.3%-2.5%. The least determination limits were 20 ng/L and 5 ng/L for BPA and BPS, respectively. Conclusion The established method is simple, sensitive and has good repeatability, which is suitable for the determination of BPA and BPS in bottled drinking water.

关 键 词：双酚A 双酚S 超高效液相色谱-串联质谱法 固相萃取 瓶装饮用水 

分 类 号：O657.63[理学—分析化学] R123.1[理学—化学]