PMID- 23786001
OWN - NLM
STAT- MEDLINE
DCOM- 20141219
LR  - 20190923
IS  - 1000-8713 (Print)
IS  - 1000-8713 (Linking)
VI  - 31
IP  - 3
DP  - 2013 Mar
TI  - [Determination of thyroid hormones in milk by high performance liquid 
      chromatography-tandem mass spectrometry].
PG  - 270-4
AB  - A method of high performance liquid chromatography-tandem mass spectrometry 
      (HPLC-MS/MS) was developed for the determination of thyroid hormones in milk 
      including 3,3',5,5 '-tetraiodothyronine (T4), 3,3', 5-triiodothyronine (T3) and 
      3,3',5 '-triiodothyronine (rT3). The sample was extracted with acetonitrile and 
      centrifuged, then the up layer was alkalized with concentrated ammonia water and 
      cleaned up with a Cleanert PAX cartridge. The chromatographic separation was 
      carried out on a Zorbax Eclipse XDB-C18 column (150 mm x 2.1 mm, 3.5 micro m) 
      with the mobile phase of 37% water containing 0.1% (v/v) acetic acid and 63% of 
      methanol with an isocratic elution mode at a flow rate of 0. 3 mL/min. The mass 
      spectrometry detection was performed in positive electrospray ionization and 
      monitored using multiple reaction monitoring (MRM) mode (m/z 652. 0/605. 5 and 
      652. 0/478. 6 for T3 and rT3; m/z 777. 7/731.7 and 777. 7/604.9 for T4; m/z 784. 
      0/737.9 and 784. 0/639.4 for T4-13C6). The analytes were identified by their 
      retention times and relative abundance ratios of the characteristic product ions, 
      and quantified by internal standard method. The method was linear with the 
      correlation coefficients ( r2 ) greater than 0. 998 in the concentration ranges 
      investigated. The limits of detection (LODs) were not more than 0.03 ng/g, and 
      the limits of quantification (LOQ) were not more than 0.1 ng/g for the analytes. 
      The recoveries were 80. 61% - 101.7% with the relative standard deviations (RSDs) 
      of 1.48% - 9.70%. The results of five real milk samples showed that the contents 
      of T3 were 0.59 - 1. 30 ng/g with the RSDs of 2.06% -7.70%, and T4 and rT3 
      weren't found. The method presents many merits including simple sample 
      pretreatment, high sensitivity, good reproducibility and unequivocal confirmation 
      and quantification for the analytes. It could be used to monitor the levels of 
      thyroid hormones in the milk for safety quality evaluation.
FAU - Wang, Zongyi
AU  - Wang Z
AD  - Beijing Key Laboratory of Agricultural Products Safety Detection and Control, 
      College of Food Science and Engineering, Beijing University of Agriculture, 
      Beijing 102206. China.
FAU - Yang, Dingzhong
AU  - Yang D
FAU - Ji, Mengyao
AU  - Ji M
FAU - Jia, Changxi
AU  - Jia C
FAU - Huang, Manqing
AU  - Huang M
LA  - chi
PT  - English Abstract
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
PL  - China
TA  - Se Pu
JT  - Se pu = Chinese journal of chromatography
JID - 9424804
RN  - 0 (Thyroid Hormones)
RN  - 06LU7C9H1V (Triiodothyronine)
RN  - Q51BO43MG4 (Thyroxine)
SB  - IM
MH  - Animals
MH  - Cattle
MH  - Chromatography, High Pressure Liquid/*methods
MH  - Food Safety/methods
MH  - Milk/*chemistry
MH  - Tandem Mass Spectrometry/*methods
MH  - Thyroid Hormones/*analysis
MH  - Thyroxine/analysis
MH  - Triiodothyronine/analysis
EDAT- 2013/06/22 06:00
MHDA- 2014/12/20 06:00
CRDT- 2013/06/22 06:00
PHST- 2013/06/22 06:00 [entrez]
PHST- 2013/06/22 06:00 [pubmed]
PHST- 2014/12/20 06:00 [medline]
AID - 10.3724/sp.j.1123.2012.10038 [doi]
PST - ppublish
SO  - Se Pu. 2013 Mar;31(3):270-4. doi: 10.3724/sp.j.1123.2012.10038.