[Determination of thiourea dioxide in lotus seed paste fillings by solid phase extraction-liquid chromatography-tandem mass spectrometry].
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 x 2.1 mm, 3.5 microm) 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 - 1 000 microg/L. The limit of detection (LOD) and limit of quantitation (LOQ) of this method were 8.0 microg/kg and 30.0 microg/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.
Hui
H
Wang
Xiwen
X
Zeng
Xiaotu
X
Chang
Xinkai
X
Peng
Lixin
L
Xia
Yiwei
Y
Li
D002851:Chromatography, High Pressure Liquid; D000070116:Lotus; D012639:Seeds / Q000737:chemistry*; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry; D013890:Thiourea / Q000031:analogs & derivatives* / Q000032:analysis
C047256:thiourea dioxide; D013890:Thiourea