色谱2017，Vol.35Issue(9)：980-986,7.DOI:10.3724/SP.J.1123.2017.06003
固相萃取-超高效液相色谱-高分辨质谱法快速测定食用油中4种酚类环境雌激素残留
Rapid determination of four phenolic environmental estrogen residues in cooking oil by ultra-performance liquid chromatography-high resolution mass spectrometry coupled with solid-phase extraction
摘要
Abstract
A fast, sensitive and accurate method for the determination of trace bisphenol S (BPS), bisphenol F (BPF), bisphenol A (BPA) and 4-nonylphenol (4-NP) in cooking oil sam-ples was developed by ultra-performance liquid chromatography-high resolution mass spectrom-etry ( UPLC-HRMS ) coupled with solid-phase extraction ( SPE ) . Cooking oil samples were extracted by acetonitrile, then the supernatant was purified by SLC SPE cartridges. The chrom-atographic separation was carried out on a Waters ACQUITY UPLC HSS T3 column ( 100 mm × 2. 1 mm, 1. 8 μm) with a linear gradient elution procedure using 0. 05% ( v/v) triethanolamine aqueous solution and methanol as mobile phases. The quantification analysis was operated in a negative electrospray ion ( ESI-) source mode under the selected ion monitoring ( SIM ) mode with internal standard method. The four target analytes showed good linearity with correlation coefficients ( r) greater than 0. 999. The limits of detection ( LODs, S/N=3) and limits of quan-tification (LOQs, S/N=10) were in the ranges of 0. 03-0. 11 μg/kg and 0. 10-0. 36 μg/kg, respectively. The recoveries of the four target analytes spiked in oil samples were in the range of 86. 3%-96. 1% at spiked levels of 1. 0, 10. 0 and 80. 0μg/kg, respectively, while the relative standard deviations ( RSDs) were in range of 2. 2%-8. 8% ( n=6) . No significant matrix inter-ference was found in this method. The proposed method is simple and fast. It can be applied for the rapid determination of trace BPS, BPF, BPA, and 4-NP in cooking oil samples.关键词
超高效液相色谱-高分辨质谱/固相萃取/酚类环境雌激素/双酚S/双酚F/双酚A/4-壬基酚/食用油Key words
ultra-performance liquid chromatography-high resolution mass spectrometry ( UPLC-HRMS)/solid-phase extraction ( SPE)/phenolic environmental estrogens/bisphenol S (BPS)/bisphenol F (BPF)/bisphenol A (BPA)/4-nonylphenol (4-NP)/cooking oil分类
化学化工引用本文复制引用
潘胜东,何仟,陈晓红,王立,邱巧丽,金米聪..固相萃取-超高效液相色谱-高分辨质谱法快速测定食用油中4种酚类环境雌激素残留[J].色谱,2017,35(9):980-986,7.基金项目
浙江省医药卫生平台骨干项目(2015RCB023) （2015RCB023）
浙江省医药卫生平台重点项目(2014ZDA021) （2014ZDA021）
宁波市自然科学基金项目(2016A610178) （2016A610178）
浙江省公共卫生应急检测关键技术重点实验室开放基金.Zhejiang Provincial Medical Health Platform Backbone Project (No.2015RCB023) （No.2015RCB023）
Zhejiang Provincial Medical Health Platform Key Project (No.2014ZDA021) （No.2014ZDA021）
Ningbo Natural Science Foundation of China (No.2016A610178) （No.2016A610178）
Opening Foundation of Key Laboratory of Key Technologies of Emergency Detection for Public Health of Zhejiang Province. （）
