色谱

色谱 ›› 2017, Vol. 35 ›› Issue (9): 980-986.DOI: 10.3724/SP.J.1123.2017.06003

• 研究论文 • 上一篇    下一篇

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

潘胜东1, 何仟2, 陈晓红1, 王立1, 邱巧丽1, 金米聪1   

  1. 1. 宁波市疾病预防控制中心, 浙江省微量有毒化学物健康风险评估技术研究重点实验室, 宁波市毒物研究与控制重点实验室, 浙江 宁波 315010;
    2. 中国疾病预防控制中心, 职业卫生与中毒控制所, 北京 100050
  • 收稿日期:2017-06-01 出版日期:2017-09-08 发布日期:2017-09-15
  • 通讯作者: 金米聪,E-mail:jmcjc@163.com.
  • 基金资助:

    浙江省医药卫生平台骨干项目（2015RCB023）；浙江省医药卫生平台重点项目（2014ZDA021）；宁波市自然科学基金项目（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.

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

PAN Shengdong1, HE Qian2, CHEN Xiaohong1, WANG Li1, QIU Qiaoli1, JIN Micong1   

  1. 1. Zhejiang Provincial Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals, Ningbo Key Laboratory of Poison Research and Control, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China;
    2. National Institute of Occupational Health and Poison Control, Chinese Center for Disease Control and Prevention, Beijing 100050, China
  • Received:2017-06-01 Online:2017-09-08 Published:2017-09-15
  • Supported by:

    Zhejiang Provincial Medical Health Platform Backbone Project (No. 2015RCB023); Zhejiang Provincial Medical Health Platform Key Project (No. 2014ZDA021); Ningbo Natural Science Foundation of China (No. 2016A610178); Opening Foundation of Key Laboratory of Key Technologies of Emergency Detection for Public Health of Zhejiang Province.

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摘要：

建立了固相萃取-超高效液相色谱-高分辨质谱（SPE-UPLC-HRMS）快速测定食用油中4种痕量酚类环境雌激素（双酚S（BPS）、双酚F（BPF）、双酚A（BPA）和4-壬基酚（4-NP））的分析方法。食用油样品经乙腈涡旋提取和SLC玻璃固相萃取小柱净化后，以0.05%（v/v）三乙醇胺和甲醇溶液为流动相进行梯度洗脱，采用Waters ACQUITY UPLC HSS T3色谱柱（100 mm×2.1 mm， 1.8 μm）进行分离，在电喷雾离子源负离子模式（ESI-）和选择性离子监测（SIM）模式下进行检测，内标法定量。4种目标物在各自的范围内有良好的线性关系，相关系数（r）>0.999。方法的检出限（LOD， S/N=3）和定量限（LOD， S/N=10）分别为0.03~0.11 μg/kg和0.10~0.36 μg/kg。在1.0、10.0和80.0 μg/kg 3个加标水平下，4种目标物的加标回收率为86.3%~96.1%，相对标准偏差（RSD）为2.2%~8.8%（n=6）。基质效应实验表明方法在低、中、高3个浓度水平下均无明显的基质干扰。该法简便、快速，能用于食用油中双酚S、双酚F、双酚A和4-壬基酚残留的快速检测。

关键词: 4-壬基酚, 超高效液相色谱-高分辨质谱, 酚类环境雌激素, 固相萃取, 食用油, 双酚A, 双酚F, 双酚S

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 samples was developed by ultra-performance liquid chromatography-high resolution mass spectrometry (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 chromatographic 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 quantification (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 80.0 μg/kg, respectively, while the relative standard deviations (RSDs) were in range of 2.2%-8.8% (n=6). No significant matrix interference 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.

Key words: 4-nonylphenol (4-NP), bisphenol A (BPA), bisphenol F (BPF), bisphenol S (BPS), cooking oil, phenolic environmental estrogens, solid-phase extraction (SPE), ultra-performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS)

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