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

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

中文摘要:

      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-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。

英文摘要:

      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.