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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 35, Number 3
BKCSDE 35(3)
March 20, 2014 

Development of Isotope Dilution LC-MS/MS Method for Accurate Determination of Arsenobetaine in Oyster Certified Reference Material
Woo Young Lee, Yong-Hyeon Yim, Euijin Hwang, Youngran Lim, Tae Kyu Kim*, Kyoung-Seok Lee*
Arsenobetaine, Speciation analysis, Certified reference material, Isotope dilution mass spectrometry, HILIC-LC-MS/MS
An isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) method has been developed and applied to the determination of arsenobetaine (AsB, (CH3)3 +AsCH2COO−) from oyster candidate certified reference material (CRM). The exact matching isotope dilution approach was adopted for accurate determination of AsB using 13C2-labeled AsB as an internal standard. Efficiencies of different AsB extraction methods were evaluated using a codfish reference material and a simple sonication method was selected as the method of choice for the certification of the oyster candidate CRM. The hydrophilic interaction liquid chromatography (HILIC) combined with electrospray ionization tandem mass spectrometry (ESI/MS/ MS) in selected reaction monitoring (SRM) mode was optimized for adequate chromatographic retention and robust quantification of AsB from codfish and oyster samples. By analyzing 12 subsamples taken from each 12 bottles systematically selected from the whole oyster CRM batch, the certified value of AsB was determined as 6.60 mg·kg−1 ± 0.31 mg·kg−1 and it showed excellent between-bottle homogeneity of less than 0.42%, which is represented by relative standard deviation of 12 bottles from the CRM batch. The major source of uncertainty was the certified value of the AsB standard solution.
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