Jin Yushen, Xing Yang, Xu Kaixin, Niu Yumin, Shao Bing
Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Prevention and Control, Beijing 100013, China.
Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Prevention and Control, Beijing 100013, China School of Public Health, Capital Medical University, Beijing 100069, China.
Wei Sheng Yan Jiu. 2025 May;54(3):510-519. doi: 10.19813/j.cnki.weishengyanjiu.2025.03.024.
A method based on QuEChERS and ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was established for the detection of 27 perfluoroalkyl substances(PFASs) in pork.
Pork samples were extracted with acetonitrile-water(8∶2, V/V), and the supernatant was purified with 100 mg primary secondary amine(PSA) and 40 mg octadecylsilyl(C18). Separation was performed using an Ascentis~(TM) Express F5(2.1 mm × 150 mm, 2 μm) chromatographic column, and detection was carried out using UPLC-MS/MS with internal standard quantification.
The 27 PFASs exhibited good linearity in the range of 0.01-50 μg/L, with limit of detection(LOD) ranging from 0.004 to 0.044 μg/L and limit of quantification(LOQ) ranging from 0.015 to 0.145 μg/L. The intra-day and inter-day precision were determined at a spiking level of 2LOQ, with a recovery rate of 72.4%-109.7% and 78.6%-110.7%, an intra-day relative standard deviation(RSD) of 1.2%-9.6%(n=6), and an inter-day RSD of 1.0%-13.8%(n=5), respectively. Using this method, 52 pork samples from Beijing markets were tested, and the result showed that all 26 PFASs compounds, except perfluorooctanesulfonamide(PFOSA), were ubiquitous and accumulated to varying degrees in pork.
This method is simple, time-saving, and has high accuracy, sensitivity, and reliability, making it suitable for simultaneous determination of 27 PFASs in pork samples and applicable to routine monitoring and quality control of PFASs in pork samples.
建立一种基于QuEChERS和超高效液相色谱 - 串联质谱法（UPLC-MS/MS）检测猪肉中27种全氟烷基物质（PFASs）的方法。
猪肉样品用乙腈 - 水（8∶2，V/V）提取，上清液用100 mg 伯仲胺（PSA）和40 mg十八烷基硅烷（C18）净化。采用Ascentis™ Express F5（2.1 mm×150 mm，2 μm）色谱柱进行分离，UPLC-MS/MS内标法定量检测。
27种PFASs在0.01 - 50 μg/L范围内线性良好，检出限（LOD）为0.004 - 0.044 μg/L，定量限（LOQ）为0.015 - 0.145 μg/L。在2LOQ加标水平下测定日内和日间精密度，回收率分别为72.4% - 109.7%和78.6% - 110.7%，日内相对标准偏差（RSD）为1.2% - 9.6%（n = 6），日间RSD为1.0% - 13.8%（n = 5）。用该方法检测北京市场的52份猪肉样品，结果表明除全氟辛烷磺酰胺（PFOSA）外的26种PFASs化合物在猪肉中普遍存在且有不同程度的蓄积。
该方法简便、省时，具有较高的准确度、灵敏度和可靠性，适用于猪肉样品中27种PFASs的同时测定，可应用于猪肉样品中PFASs的常规监测和质量控制。
