Wei sheng yan jiu = Journal of hygiene research · 2025
[Determination of 27 perfluoroalkyl substances in pork by ultra-high performance liquid chromatography-tandem mass spectrometry].
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Jin Yushen, Xing Yang, Xu Kaixin, Niu Yumin, Shao Bing
Аннотация
OBJECTIVE: 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.
METHODS: 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.
RESULTS: 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.
CONCLUSION: 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.
METHODS: 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.
RESULTS: 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.
CONCLUSION: 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.