超高效液相色谱-串联质谱法测定人体尿液中6种双酚类化合物

Determination of six bisphenols in human urine by ultra-high performance liquid chromatography-tandem mass spectrometry

目的开发并验证测定尿液中6种双酚类化合物(双酚S、双酚F、双酚A、2,2′-亚甲基双酚、双酚AF、双酚AP)的固相萃取-超高效液相色谱-串联质谱检测方法。方法尿样酶解后,经WAX固相萃取柱快速净化和提取目标物,以水和甲醇为流动相在色谱柱ACQUITY BEH C_(18)(2.1 mm×100 mm,1.7μm)上进行分离,最后在电喷雾负离子模式下进行多反应监测,内标法进行定量。结果目标化合物在0.1~50.0 ng/mL的范围内相关系数(r)均大于0.998,线性良好,检出限均低于0.1 ng/mL。3个加标浓度(0.5、5.0和50.0 ng/mL)下的目标化合物回收率均在80%~120%,相对标准偏差小于20%(n=5)。对标准参考物质进行检测,检出浓度在参考范围内。结论该方法能够对尿液中6种双酚类化合物进行快速、准确的检测,适用于人体尿液中双酚类化合物的痕量分析。

OBJECTIVE To develop and validate a solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry method for the determination of six bisphenols(bisphenol S,bisphenol F,bisphenol A,2,2′-methylenediphenol,bisphenol AF,bisphenol AP)in urine.METHODS After enzymolysis of urine sample,the target substances were quickly purified and extracted by WAX solid phase extraction column.On ACQUITY BEH C_(18)column(2.1 mm×100 mm,1.7μm),the mobile phase of water and methanol was used to separate.Finally,multi-reaction detection was carried out under electrospray negative ion scanning,and quantification was carried out by internal standard method.RESULTS The correlation coefficients(r)of the target compounds were all more than 0.998 in the range of 0.1-50.0 ng/mL,the linearity was good,and the detection limits were all lower than 0.1 ng/mL.The recoveries of the three standard concentrations(0.5,5.0 and 50.0 ng/mL)were all between 80%and 120%,and the relative standard deviation was less than 20%(n=5).The standard reference material was detected and the concentration was within the reference range.CONCLUSION This method can be used to detect six bisphenols in urine quickly and accurately,is suitable for the trace analysis of bisphenol compounds in human urine.