【摘要】 目的建立同时测定水果中双酚A、17β-雌二醇、雌酮、雌三醇、炔雌醇、己烯雌酚、4-辛基酚和4-n-壬基酚的高效液相色谱-串联质谱法。方法样品经乙腈超声提取2次,Oasis HLB固相萃取柱净化,提取液氮吹至干,残渣用甲醇溶解。待测物以乙腈-甲醇(4∶1,V/V)与0.1%氨水为流动相,经ACQUITY UPLCBEH C18色谱柱(2.1 mm×100 mm,1.7μm)梯度洗脱分离后,进行HPLC-MS/MS多反应监测模式(MRM)的定性及定量分析,外标法定量。结果 8种环境雌激素能与杂质较好分离,在5~100μg/L范围内线性良好(均r≥0.99)。方法检出限为0.17~0.51μg/kg,定量限为1.33~2.55μg/kg,加标回收率为67.77%~110.49%,RSD为1.08%~12.74%。应用该方法对实际样品进行检测,均有微量双酚A检出,大部分检测到4-n-壬基酚和炔雌醇,部分检测到17β-雌二醇,其余4种环境雌激素均未检出。结论本方法快速、灵敏、准确,适用于水果中8种环境雌激素的定量及确证分析。更多还原

【Abstract】 Objective To establish a high performance liquid chromatography-mass spectrometry( HPLC-MS / MS)method for the simultaneous determination of 8 environmental estrogens,including bisphenol A,4-n-nonylphenol,estrone,17β-estradio,estradiol,ethinyl estradiol,4-octylpheno and diethy lstilbestrol in fruits. Methods Fruit samples were ultrasonic extracted by acetonitrile and cleaned up on a HLB solid phase extraction column. The extract was evaporated to dryness under nitrogen,and the residue was redissolved in methanol. The gradient elution of 8 environmental estrogens was carried out by a ACQUITY UPLC BEH C18column( 2. 1 mm × 100 mm,1. 7 μm) using acetonitrile-methanol( 4 ∶ 1,V / V) and 0. 1% ammonia aqueous solution as the mobile phase. The target compounds were confirmed and quantified by HPLC-MS / MS under multiple reaction monitoring( MRM) mode with external standard method. Results 8 environmental estrogens and impurity could be well separated,and it showed good linearity in the range of 5-100 μg / L( each r≥0. 99).The detection limit of the method was 0. 17-0. 51 μg / kg,the limit of quantification was 1. 33-2. 55 μg / kg,the average recovery was 67. 77%-110. 49%,and the precision was 1. 08%-12. 74%. The method was applied to fruit samples,bisphenol A was detected in all samples,most samples were detected 4-n-nonylphenol and ethinyl estradiol,some were detected 17β-estradiol and remaining 4 environmental estrogens were not detected. Conclusion The method is rapid,sensitive and accurate,and was suitable for the determination and confirmation of 8 environmental estrogens in fruit.更多还原