PMID- 38093539
OWN - NLM
STAT- MEDLINE
DCOM- 20231216
LR  - 20231216
IS  - 1872-2059 (Electronic)
IS  - 1000-8713 (Print)
IS  - 1000-8713 (Linking)
VI  - 41
IP  - 12
DP  - 2023 Dec
TI  - [Determination of 14 perfluoroalkyl substances in Chinese mitten crab by 
      multi-plug filtration cleanup coupled with ultra-performance liquid 
      chromatography-tandem mass spectrometry].
PG  - 1095-1105
LID - 10.3724/SP.J.1123.2023.07017 [doi]
AB  - Perfluoroalkyl substances (PFASs) have become a new food-safety problem. Dietary 
      intake is a major pathway of human exposure to PFASs. Chinese mitten crab 
      (Eriocheir sinensis) is a high-end aquaculture product popular among consumers in 
      China. Conventional extraction methods for PFASs are cumbersome and time 
      consuming, and result in incomplete purification; thus, this technique does not 
      meet the requirements for PFAS detection. Herein, an analytical strategy was 
      established for the rapid detection of 14 PFASs in Chinese mitten crab based on 
      multi-plug filtration cleanup (m-PFC) and ultra-performance liquid 
      chromatography-tandem mass spectrometry (UPLC-MS/MS). The carbon-chain length of 
      the 14 PFASs analyzed in this study ranged from 4 to 14, and they are 
      perfluorobutanoic acid (PFBA), perfluoro-n-pentanoic acid (PFPeA), 
      perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), 
      perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), perfluorodecanoic 
      acid (PFDA), perfluoroundecanoic acid (PFUnDA), perfluorododecanoic acid 
      (PFDoDA), perfluorotetradecanoic acid (PFTeDA), perfluoro-1-butane sulfonic acid 
      (PFBS), perfluoro-1-hexane sulfonic acid (PFHxS), perfluoro-1-octane sulfonic 
      acid (PFOS), and perfluoro-1-decanesulfonate (PFDS). The m-PFC column was 
      prepared using carboxy-based multiwalled carbon nanotubes, and used to reduce the 
      interference of sample impurities. The samples were extracted with 5 mL of 0.1% 
      formic acid aqueous solution, 15 mL of acetonitrile and extraction salt (2 g 
      Na(2)SO(4) and 2 g NaCl). The supernatant (10 mL) was purified using the m-PFC 
      column, concentrated to near dryness under nitrogen, and then redissolved in 1 mL 
      of methanol. Finally, the sample solution was filtered through a 0.22 mum 
      polypropylene syringe filter for UPLC-MS/MS analysis. The target analytes were 
      separated using a Shimadzu Shim-pack G1ST-C18 chromatographic column (100 mmx2.1 
      mm, 2 mum) using methanol (A) and 5 mmol/L ammonium acetate aqueous solution (B) 
      as the mobile phases via gradient elution. The linear gradient program were as 
      follows: 0-0.5 min, 10%A-35%A; 0.5-3 min, 35%A-60%A; 3-5 min, 60%A-100%A; 5-6.5 
      min, 100%A; 6.5-7 min, 100%A-10%A. The target analytes were analyzed using 
      negative electrospray ionization in multiple-reaction monitoring mode, and 
      quantitative analysis was performed using the internal standard method. In this 
      study, we optimized the mobile-phase system as well as the extraction solvent, 
      time, volume, and salt. The 14 PFASs exhibited good peak shapes and sensitivities 
      when the 5 mmol/L ammonium acetate solution-methanol system was used as the 
      mobile phase. Compared with acetonitrile or methanol alone, the extraction 
      efficiencies of the 14 PFASs were significantly improved when 5 mL of 0.1% formic 
      acid aqueous solution was added, followed by 15 mL of acetonitrile. The 
      extraction efficiencies of the 14 PFASs did not differ significantly when the 
      extraction time was within 3-15 min. The extraction salt (MgSO(4), Na(2)SO(4), 
      NaCl, (NH(4))(2)SO(4), and Na(2)SO(4)+NaCl) significantly affected the extraction 
      efficiencies of the 14 PFASs. The highest extraction efficiencies of the 14 
      PFASs, which ranged from 47.9% to 121.9%, were obtained when Na(2)SO(4)+NaCl was 
      used as the extraction salt. Under the optimal experimental conditions, good 
      linearities (R(2)=0.998-0.999) were obtained for seven PFASs (PFBS, PFHxA, PFHpA, 
      PFHxS, PFDA, PFDoDA, PFTeDA) at 0.10-100 mug/L, and seven PFASs (PFBA, PFPeA, 
      PFOA, PFOS, PFNA, PFUnDA, PFDS) at 0.50-100 mug/L. The average spiked recoveries 
      for the 14 PFASs in Chinese mitten crabs at three levels ranged from 73.1% to 
      120%, with relative standard deviations (RSDs) in the range of 1.68%-19.5%(n=6). 
      The limits of detection (LODs) and quantification (LOQs) of the 14 PFASs were in 
      the range of 0.03-0.15 and 0.10-0.50 mug/kg, respectively. The developed method 
      was applied to the analysis of crab samples collected from three farms in 
      Shanghai, and PFASs with total concentrations of 3.52-37.77 mug/kg were detected 
      in all samples. The detection frequencies for PFDA, PFUnDA, PFDoDA, PFTeDA, and 
      PFOS were 100%. PFDA, PFUnDA, PFOS, and PFDoDA were the most abundant congeners, 
      accounting for 31.2%, 30.6%, 15.0%, and 10.9%, respectively, of the 14 PFASs 
      detected. The proposed method is simple, efficient, accurate, and suitable for 
      the rapid analysis of 14 PFASs in Chinese mitten crabs.
FAU - Wang, Xianli
AU  - Wang X
AD  - Institute for Agro-food Standards and Testing Technology, Shanghai Academy of 
      Agricultural Sciences, ShanghaiAgricultural Product Quality and Safety Evaluation 
      Technical Service Platform, Shanghai 201403, China.
FAU - Rao, Qinxiong
AU  - Rao Q
AD  - Institute for Agro-food Standards and Testing Technology, Shanghai Academy of 
      Agricultural Sciences, ShanghaiAgricultural Product Quality and Safety Evaluation 
      Technical Service Platform, Shanghai 201403, China.
FAU - Zhang, Qicai
AU  - Zhang Q
AD  - Institute for Agro-food Standards and Testing Technology, Shanghai Academy of 
      Agricultural Sciences, ShanghaiAgricultural Product Quality and Safety Evaluation 
      Technical Service Platform, Shanghai 201403, China.
FAU - DU, Penghui
AU  - DU P
AD  - Institute for Agro-food Standards and Testing Technology, Shanghai Academy of 
      Agricultural Sciences, ShanghaiAgricultural Product Quality and Safety Evaluation 
      Technical Service Platform, Shanghai 201403, China.
FAU - Song, Weiguo
AU  - Song W
AD  - Institute for Agro-food Standards and Testing Technology, Shanghai Academy of 
      Agricultural Sciences, ShanghaiAgricultural Product Quality and Safety Evaluation 
      Technical Service Platform, Shanghai 201403, China.
LA  - chi
PT  - English Abstract
PT  - Journal Article
PL  - China
TA  - Se Pu
JT  - Se pu = Chinese journal of chromatography
JID - 9424804
RN  - 0 (perfluoroundecanoic acid)
RN  - RRE756S6Q2 (ammonium acetate)
RN  - 0YIW783RG1 (formic acid)
RN  - 451W47IQ8X (Sodium Chloride)
RN  - Y4S76JWI15 (Methanol)
RN  - 0 (Nanotubes, Carbon)
RN  - 0 (Fluorocarbons)
RN  - 0 (perfluorotetradecanoic acid)
RN  - 947VD76D3L (perfluorooctanoic acid)
RN  - 6P60ZBK0QL (perfluorooctane)
RN  - 375-95-1 (perfluoro-n-nonanoic acid)
RN  - 0 (Sulfonic Acids)
RN  - 0 (Acetonitriles)
SB  - IM
MH  - Humans
MH  - Tandem Mass Spectrometry
MH  - Chromatography, Liquid
MH  - Sodium Chloride/analysis
MH  - Methanol
MH  - *Nanotubes, Carbon/analysis
MH  - China
MH  - *Fluorocarbons/analysis
MH  - Sulfonic Acids/analysis
MH  - Acetonitriles
MH  - Chromatography, High Pressure Liquid
MH  - Solid Phase Extraction
PMC - PMC10719808
OTO - NOTNLM
OT  - Chinese mitten crab
OT  - multi-plug filtration cleanup (m-PFC)
OT  - perfluoroalkyl substances (PFASs)
OT  - ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)
EDAT- 2023/12/14 06:42
MHDA- 2023/12/17 10:19
PMCR- 2023/12/08
CRDT- 2023/12/14 02:05
PHST- 2023/12/17 10:19 [medline]
PHST- 2023/12/14 06:42 [pubmed]
PHST- 2023/12/14 02:05 [entrez]
PHST- 2023/12/08 00:00 [pmc-release]
AID - 10.3724/SP.J.1123.2023.07017 [doi]
PST - ppublish
SO  - Se Pu. 2023 Dec;41(12):1095-1105. doi: 10.3724/SP.J.1123.2023.07017.