PMID- 35080168
OWN - NLM
STAT- MEDLINE
DCOM- 20220127
LR  - 20220915
IS  - 1872-2059 (Electronic)
IS  - 1000-8713 (Print)
IS  - 1000-8713 (Linking)
VI  - 40
IP  - 2
DP  - 2022 Feb 8
TI  - [Determination of fipronil and its metabolites in livestock and poultry liver by 
      high performance liquid chromatography-tandem mass spectrometry with dispersive 
      solid phase extraction].
PG  - 206-211
LID - 10.3724/SP.J.1123.2021.04007 [doi]
AB  - The residues of fipronil and its metabolites, namely fipronil-desulfinyl, 
      fipronil-sulfone, and fipronil-sulfide, have attracted increasing attention since 
      the European egg contamination incident. In this study, by optimizing the 
      pretreatment method and chromatographic conditions, a simple extraction method 
      coupled with high performance liquid chromatography-tandem mass spectrometry was 
      developed for the simultaneous determination of fipronil and its metabolites, 
      including fipronil-desulfinyl, fipronil-sulfone, and fipronil-sulfide, in 
      livestock and poultry liver. The optimal pretreatment method for fipronil and its 
      metabolites was determined by comparing the recoveries obtained with different 
      extraction solvents (methanol, acetonitrile, acetone, and ethyl acetate), and by 
      purification with N-propyl ethylenediamine (PSA) and octadecylsilane (C18). The 
      samples were extracted with 10 mL acetonitrile, then purified with 150 mg PSA and 
      100 mg C18, following which the extracted solutions were directly injected for 
      analysis. Separation was performed on an Agilent ZORBAX SB-C18 column (150 mmx2.1 
      mm, 3.5 mum) with gradient elution using acetonitrile and water as the mobile 
      phases. The target compounds were detected by electrospray ionization (ESI) in 
      the negative mode under multiple reaction monitoring, and quantified by the 
      external standard method with matrix-matched standard correction curves. The 
      results indicated that the linear ranges for the four compounds ranged from 0.1 
      mug/L to 10.0 mug/L with correlation coefficients (r(2)) higher than 0.995. The 
      limit of detection was 0.2 mug/kg and limit of quantitation was 0.5 mug/kg. The 
      average recoveries were between 81.1% and 99.8% at three spiked levels of 0.5, 
      1.0, and 10 mug/kg, with relative standard deviations (RSDs) of 6.1%-11.7%. The 
      matrix effect experiment showed that fipronil and its metabolites had matrix 
      inhibition effects. Matrix-matched standard curve correction was performed to 
      eliminate matrix inhibition effects. The proposed method was used for the 
      analysis of 99 liver samples, where fipronil-sulfone was detected in four samples 
      with values of 1.25-2.82 mug/kg. The method is simple, sensitive, and accurate, 
      and is suitable for the determination of fipronil and its metabolites in 
      livestock and poultry liver.
FAU - Wei, Yunji
AU  - Wei Y
AD  - State Key Laboratory of Feed Safety Testing (Huai'an), Huai'an Customs, Huai'an 
      223001, China.
FAU - Bao, Huimei
AU  - Bao H
AD  - Jiangsu Food & Pharmaceutical Science College, Huai'an 223003, China.
FAU - He, Zhenghe
AU  - He Z
AD  - State Key Laboratory of Feed Safety Testing (Huai'an), Huai'an Customs, Huai'an 
      223001, China.
FAU - Huang, Gaoming
AU  - Huang G
AD  - Jiangsu Food & Pharmaceutical Science College, Huai'an 223003, China.
FAU - Feng, Min
AU  - Feng M
AD  - State Key Laboratory of Feed Safety Testing (Huai'an), Huai'an Customs, Huai'an 
      223001, China.
FAU - Zhu, Zhenyi
AU  - Zhu Z
AD  - State Key Laboratory of Feed Safety Testing (Huai'an), Huai'an Customs, Huai'an 
      223001, China.
FAU - He, Jian
AU  - He J
AD  - State Key Laboratory of Feed Safety Testing (Huai'an), Huai'an Customs, Huai'an 
      223001, China.
LA  - chi
PT  - Journal Article
PL  - China
TA  - Se Pu
JT  - Se pu = Chinese journal of chromatography
JID - 9424804
RN  - 0 (Pyrazoles)
RN  - QGH063955F (fipronil)
SB  - IM
MH  - Animals
MH  - Chromatography, High Pressure Liquid
MH  - Liver
MH  - *Livestock
MH  - Poultry
MH  - Pyrazoles
MH  - Solid Phase Extraction
MH  - *Tandem Mass Spectrometry
PMC - PMC9404094
OTO - NOTNLM
OT  - dispersive solid phase extraction (dSPE)
OT  - fipronil and its metabolites
OT  - high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)
OT  - livestock and poultry liver
EDAT- 2022/01/27 06:00
MHDA- 2022/01/28 06:00
PMCR- 2022/02/08
CRDT- 2022/01/26 05:34
PHST- 2022/01/26 05:34 [entrez]
PHST- 2022/01/27 06:00 [pubmed]
PHST- 2022/01/28 06:00 [medline]
PHST- 2022/02/08 00:00 [pmc-release]
AID - 1000-8713-40-2-206 [pii]
AID - 10.3724/SP.J.1123.2021.04007 [doi]
PST - ppublish
SO  - Se Pu. 2022 Feb 8;40(2):206-211. doi: 10.3724/SP.J.1123.2021.04007.