固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中6种雌激素

Determination of six estrogens in honey using ultra performance liquid chromatography-tandem mass spectrometry

建立了固相萃取-超高效液相色谱-串联质谱对蜂蜜中雌酮、雌二醇、雌三醇、炔雌醇、己烷雌酚、双酚A等6种雌激素的测定方法。蜂蜜样品用固相萃取柱富集及净化,有效降低了基质的干扰。以乙腈:甲醇(4:1,V/V)和0. 1%氨水溶液作为流动相,经BEH RP18色谱柱分离,采用电喷雾离子源、质谱多反应监测和负离子扫描模式,实现了蜂蜜中6种雌激素的同时检测。6种雌激素的加标回收率为78. 5%～112. 9%,RSD为0. 66%～8. 9%。雌酮、雌二醇、雌三醇、炔雌醇、己烷雌酚、双酚A的方法检出限和定量限分别为0. 04～0. 19μg/kg和0. 15～0. 62μg/kg。方法适用于蜂蜜中雌激素的分析和检测。

A method for the determination of estrone(E1),17β-estradiol(E2),estriol(E3),17α-ethynylestradiol(EE2),hexoestrolum(HE),bisphenol A(BPA)in honey samples was developed based on UPLC-MS/MS.Solid phase extraction was used for extraction and purification so as to efficiently minimize the matrix effect.The chromatographic separation was under the mobile phase of0.1%ammonia/acetonitrile-methanol(4:1,V/V)using a BEH RP18 column.The quantification analysis was operated under the multiple reaction monitoring mode in a negative electrospray ion source mode.The recoveries of the six target compounds in honey samples were in the range of 78.5%-112.9%and the relative standard deviations(RSDs)were in the range of 0.66%-8.9%.The limits of detection and limits of quantification were in the ranges of 0.04-0.19μg/kg and 0.15-0.62μg/kg,respectively.The proposed method has been successfully applied to the determination of E1,E2,E3,EE2,HE and BPA residues in honey samples.