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
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-D4和BPS-13C12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 C18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1~50 μg/L范围内线性良好, BPS在0.2~10 μg/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 of bisphenol 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.
标题：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
英文标题：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 辽宁省疾病预防控制中心沈阳110005
李延升 辽宁省疾病预防控制中心沈阳110005
韩晓鸥 辽宁省疾病预防控制中心沈阳110005
陈曦 辽宁省疾病预防控制中心沈阳110005
高岩 辽宁省疾病预防控制中心沈阳110005
中文关键词: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,
英文关键词:bisphenol A,bisphenol S,ultra performance liquid chromatography-tandem mass spectrometry,solid phase extraction,bottled drinking water,
发表日期：2018-02-27
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