目的建立人血清中双酚A(BPA)和4-叔丁基苯酚(4-t-BP)的超高效液相色谱串联三重四极杆质谱测定方法。方法取200μl血清用β-葡萄糖醛酸酶水解,甲基叔丁基醚萃取,丹酰氯衍生化后,采用C18超高效液相色谱柱和含0.1%甲酸的甲醇和水流动相梯度洗脱分离,三重四极杆质谱仪测定,内标标准曲线法定量。结果 BPA和4-t-BP浓度为0.1 ng/ml~50 ng/ml时,线性关系良好,相关系数(r)均>0.995;3倍基线噪声所对应的BPA、4-t-BP的方法检出限分别为0.05 ng/ml和0.07 ng/ml。在1.0 ng/ml、2.0 ng/ml和10 ng/ml 3种加标水平下,BPA和4-tBP的加标回收率平均值分别为88%~104%、83%~96%,相对标准偏差(RSD)分别为5.9%~8.2%、6.1%~13.0%。该方法成功应用于20份实际人血清中BPA和4-t-BP的分析,并且在血清中均检出BPA,但是未检出4-t-BP。结论该方法样品前处理简单快速,而且灵敏高,准确性好,适合于大规模人群血清中BPA和4-t-BP的分析。 Objective To establish a method for the determination of bisphenol A (BPA) and 4-tert-butylphenol (4-t-BP) in human serum by tandem triple-quadrupole mass spectrometry. Methods 200 μl of serum was extracted with β-glucuronidase, extracted with methyl tert-butyl ether and dansyl chloride. The residue was separated on a C18 ultracentrifugation column and a mobile phase of methanol and water containing 0.1% formic acid. , Triple quadrupole mass spectrometry, internal standard curve method. Results When the concentrations of BPA and 4-t-BP were between 0.1 ng / ml and 50 ng / ml, the linear relationship was good with the correlation coefficients (r)> 0.995. The BPA and 4-t-BP The limits of detection were 0.05 ng / ml and 0.07 ng / ml, respectively. The average recoveries of BPA and 4-tBP at the three spiked levels of 1.0 ng / ml, 2.0 ng / ml and 10 ng / ml were 88% -104% and 83% -96%, respectively. The relative standard Deviation (RSD) were 5.9% ~ 8.2%, 6.1% ~ 13.0%. This method was successfully applied to the analysis of BPA and 4-t-BP in 20 real human serums, and BPA was detected in serum but no 4-t-BP was detected. Conclusion The method of sample preparation is simple, rapid, sensitive, accurate and suitable for the analysis of BPA and 4-t-BP in serum of large-scale population.