Determination of 71 Kinds of Per-and Polyfluoroalkyl Substances in Eckloniae Thallus by QuEChERS-Liquid Chromatography-Tandem Mass Spectrometry
10.19756/j.issn.0253-3820.241471
- VernacularTitle:QuEChERS-液相色谱-串联质谱法测定中药材昆布中71种全/多氟化合物残留
- Author:
Dan-Rui TANG
1
;
Jing SUN
;
Ling CAO
;
Dan-Yi JIANG
;
Hai-Wei SHI
;
Lu-Lu WU
Author Information
1. 南京中医药大学药学院,南京 210023;江苏省药品监督检验研究院,南京 210019
- Keywords:
Per-and polyfluoroalkyl substances;
QuEChERS;
Eckloniae Thallus;
Food-medicine homology;
Perfluoroalkyl phosphonic acids;
Neutral per-and polyfluoroalkyl substances
- From:
Chinese Journal of Analytical Chemistry
2025;53(7):1177-1185,中插9-中插25
- CountryChina
- Language:Chinese
-
Abstract:
A QuEChERS cleanup-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for simultaneous determination of traditional and emerging 71 kinds of per-and polyfluoroalkyl substances(PFAS)in Chinese herbal medicine Eckloniae Thallus.The extraction solvent employed here was 0.2%formic acid-acetonitrile with sodium chloride-anhydrous sodium sulfate(3:1,m/m)as salting-out agent,and the purification was carried out using graphitized carbon black and octadecyl-bonded silica as adsorbents.The sample separation was carried out on a Horizon C18 chromatographic column(150 mm×2.1 mm,1.6 μm)by gradient elution with 2.5 mmol/L ammonium acetate aqueous solution(containing 2.5 mmol/L acetic acid)and acetonitrile as the mobile phases.The flow rate was set at 0.4 mL/min,with an injection volume of 5 μL.The chromatographic separation of each target compound and internal standard substance could be achieved within 15 min.An electrospray ion source was utilized for simultaneous scanning of positive and negative ions under the scheduled multiple reaction monitoring(sMRM)mode,and the internal standard method was used for quantitative analysis.The results of method validations showed that the 71 kinds of PFAS had good linearity,with a correlation coefficient(r)greater than 0.997,spiked recoveries of 76.2%?122.0%and relative standard deviations(RSDs)of 5.5%?14.8%.The limits of detection were in the range of 0.3-60 ng/kg and the limits of quantification were in the range of 0.8-199 ng/kg.The developed method was used for detection of PFAS in 14 batches of Eckloniae Thallus samples,and a total of 19 kinds of PFAS were detected.The findings indicated that PFAS residues were commonly present in Eckloniae Thallus,with perfluorocarboxylic acids(PFCAs)exhibiting the highest concentrations.The method was simple,robust and efficient in preparation,sensitive in detection with high throughput,and suitable for monitoring residual PFAS compounds,including both ionic and neutral in food-medicine homology samples such as Eckloniae Thallus.