Determination of thiourea dioxide in lotus seed paste fillings by solid phase extraction-liquid chromatography-tandem mass spectrometry

doi:10.3724/SP.J.1123.2013.07015

Abstract

Abstract:

A method of solid phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) was developed to determine thiourea dioxide which was illegally added into lotus seed paste fillings. An amount of 0.05% (v/v) acetic acid was used to extract thiourea dioxide from fillings, and the BOND ELUT PLEXA column (60 mg/3 mL) was used as the SPE column to clean-up the extraction. Then, an Agilent HILIC column (100 mm×2.1 mm, 3.5 μm) was applied to separate target compounds by using the mobile phases of 0.01 mol/L ammonium acetate (pH 3.5) and acetonitrile. Qualitative and quantitative analyses were operated by the multiple reaction monitoring (MRM) mode. The calibration curve showed a good linearity for the target compound in the detection range of 10-1000 μg/L. The limit of detection (LOD) and limit of quantitation (LOQ) of this method were 8.0 μg/kg and 30.0 μg/kg, respectively. The recoveries were in the ranges of 75.3%-80.7% with the RSDs of no more than 4.83%. This proposed method was rapid, highly specific and suitable for the confirmation and quantitative determination of thiourea dioxide in lotus seed paste fillings.

Key words: liquid chromatography-tandem mass spectrometry, lotus seed paste fillings, solid phase extraction, thiourea dioxide

CLC Number:

O658

WANG Hui, ZENG Xiwen, CHANG Xiaotu, PENG Xinkai, XIA Lixin, LI Yiwei. Determination of thiourea dioxide in lotus seed paste fillings by solid phase extraction-liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2014, 32(1): 21-25.

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