超高效液相色谱-串联质谱法测定奶茶中4种烷基酚类化合物  

Determination of four kinds of alkylphenols in milk tea by ultra-high performance liquid chromatography-tandem mass spectrometry

作　　者：林胜军[1] 黄诚[1] 卢丽明[1] LIN Sheng-jun;HUANG Cheng;LU Li-ming(Zhongshan Municipal Center for Disease Control and Prevention,Zhongshan,Guangdong 528403,China)

机构地区：[1]中山市疾病预防控制中心,广东中山528403

出　　处：《中国卫生检验杂志》2019年第2期132-134,139,共4页Chinese Journal of Health Laboratory Technology

基　　金：中山市科技计划项目(2015SYF0104)

摘　　要：目的建立超高效液相色谱-串联质谱法测定奶茶中双酚A(BPA)、双酚S(BPS)、辛基酚(OP)和壬基酚(NP)的残留量。方法奶茶样品经过离心后,直接取上清液用固相萃取柱进行净化,然后用ZORBAX SB-Aq色谱柱(3. 0 mm×100 mm,1. 8μm)分离,再用甲醇和5 mmol/L乙酸铵溶液作为流动相进行梯度洗脱,最后注入到质谱仪中,以电喷雾负离子模式(ESI-)电离,多反应监测模式(MRM)进行检测。结果 BPA、BPS在2μg/L～100μg/L线性关系良好(r> 0. 999),方法的检出限(S/N=3)为0. 3μg/L、0. 01μg/L,回收率为75. 0%～86. 7%,相对标准偏差(n=6)为1. 0%～5. 8%; OP、NP在10μg/L～500μg/L线性关系良好(r> 0. 999),方法的检出限(S/N=3)为0. 7μg/L、0. 9μg/L,回收率为73. 4%～112. 0%,相对标准偏差(n=6)为1. 9%～5. 9%。结论该方法简单、灵敏、准确可靠,适用于奶茶中4种烷基酚的测定。Objective To establish a method for the determination of bisphenol A (BPA),bisphenol S (BPS),octyl phenol (OP)and nonylphenol (NP)in milk tea by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).Methods Milk tea samples were purified by solid phase extraction column after centrifugation,and then separated by ZORBAX SB-Aq column (3.0 mm×100 mm,1.8μm)and eluted,with methanol and 5mmol/L ammonium acetate solution as mobile phase.Finally,it was injected into the mass 'spectrometer that ionized in electrospray negative ion mode (ESI-)and detected in multireaction monitoring mode (MRM).Results BPA and BPS have good linearity in the range of 2μg/L-100μg/L (r >0.999);the detection limit of the method (S/N =3)were respectively 0.3μg/L and 0.01μg/L, the recovery was within 75.0%-86.7% and the relative standard deviation(n =6)was within 1.0%-5.8%.OP and NP had good linearity within 10μg/L-500μg/L (r >0.999);the detection limit of the method (S/N =3)were respectively 0.7μg/L and 0.9μg/L,the recovery was within 73.4%-112.0% and the relative standard deviation (n=6)was within 1.9%-5.9%. Conclusion The method is simple,sensitive,accurate and reliable,which is suitable for the determination of four alkylphenols in milk tea.

关 键 词：超高效液相色谱-串联质谱法 奶茶 烷基酚 

分 类 号：R155.5[医药卫生—营养与食品卫生学]