Pan Shengdong, He Qian, Chen Xiaohong, Wang Li, Qiu Qiaoli, Jin Micong
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.
National Institute of Occupational Health and Poison Control, Chinese Center for Disease Control and Prevention, Beijing 100050, China.
Se Pu. 2017 Sep 8;35(9):980-986. doi: 10.3724/SP.J.1123.2017.06003.
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 T 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 () greater than 0.999. The limits of detection (LODs, =3) and limits of quantification (LOQs, =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% (=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.
建立了一种超高效液相色谱 - 高分辨质谱(UPLC - HRMS)结合固相萃取(SPE)快速、灵敏、准确测定食用油样品中痕量双酚S(BPS)、双酚F(BPF)、双酚A(BPA)和4 - 壬基酚(4 - NP)的方法。食用油样品用乙腈萃取,然后上清液用SLC SPE小柱净化。色谱分离在Waters ACQUITY UPLC HSS T柱(100 mm×2.1 mm,1.8 μm)上进行,采用0.05%(v/v)三乙醇胺水溶液和甲醇作为流动相的线性梯度洗脱程序。定量分析在负离子电喷雾离子(ESI)源模式下的选择离子监测(SIM)模式下采用内标法进行。四种目标分析物显示出良好的线性,相关系数()大于0.999。检测限(LODs,=3)和定量限(LOQs,=10)分别在0.03 - 0.11 μg/kg和0.10 - 0.36 μg/kg范围内。在1.0、10.0和80.0 μg/kg的加标水平下,食用油样品中四种目标分析物的回收率分别在86.3% - 96.1%范围内,而相对标准偏差(RSDs)在2.2% - 8.8%范围内(=6)。该方法未发现明显的基质干扰。所提出的方法简单快速。可用于食用油样品中痕量BPS、BPF、BPA和4 - NP的快速测定。