高效液相色谱-串联质谱法测定水果中的8种环境雌激素

发布时间：2017-12-27 19:12

本文关键词：高效液相色谱-串联质谱法测定水果中的8种环境雌激素　出处：《中国食品卫生杂志》2016年04期 　论文类型：期刊论文

【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屮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。
[Abstract]:Objective to establish a HPLC simultaneous determination of bisphenol A in fruits, 17 beta estradiol, estrone, estradiol three alcohol, ethinyl estradiol and diethylstilbestrol, 4- octylphenol and nonylphenol 4-n- chromatography tandem mass spectrometry. The samples were extracted 2 times by acetonitrile and purified by Oasis HLB solid phase extraction column. The liquid nitrogen was extracted to dry, and the residue was dissolved in methanol. The analytes in methanol acetonitrile (4: 1, V/V) and 0.1% ammonia solution as mobile phase, the ACQUITY UPLC type BEH C18 column (2.1 mm * 100 mm, 1.7 m) gradient elution separation, HPLC-MS/MS multiple reaction monitoring mode (MRM) qualitative and quantitative analysis, external standard method. The results of 8 kinds of environmental estrogens can better separation and impurity, good linearity in the 5~100 g/L range (r = 0.99). The detection limit of the method is 0.17~0.51 mu g/kg, the quantitative limit is 1.33~2.55 mu g/kg, the recovery rate of adding standard is 67.77%~110.49%, and RSD is 1.08%~12.74%. The method was applied to the detection of real samples. Trace bisphenol A was detected. Most of 4-n- nonylphenol and estriol were detected. 17 beta estradiol was detected, and the remaining 4 environmental estrogens were not detected. Conclusion this method is fast, sensitive and accurate, and is suitable for quantitative and confirmatory analysis of 8 kinds of environmental estrogens in fruit.
【作者单位】：湖南师范大学医学院;华中农业大学农业微生物学国家重点实验室;
【基金】：湖南省自然科学基金项目(14JJ4028) 农业微生物学国家重点实验室开放课题(AMLKF201209) 湖南省教育厅教改项目(湘教通[2014]247号) 2016年湖南省普通高等学校教学改革研究项目湖南省研究生科研创新项目(CX2015B182)
【分类号】：R155.5;O657.63
【正文快照】： 环境雌激素(environmental estrogens,EEs)是指一类进入机体后,能够与雌激素受体结合,或者以影响细胞信号途径等其他方式模仿或部分模仿雌激素,发挥类似雌激素效应[1],干扰机体的内分泌物质的正常功能,破坏机体内环境稳定的化合物[2],包括人工合成化合物及植物天然雌激素,属于

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