Citation: LI Hanke, YI Lezhou, TAN Zhixian, DING Zhiyong, HUANG Ningshan, HUANG Lina, MA Tongmei. Determination of monomethyltin migration from toys by gas chromatography-mass spectrometry and confirmation of its false positive[J]. Chinese Journal of Chromatography, ;2018, 36(11): 1181-1188. doi: 10.3724/SP.J.1123.2018.06004 shu

Determination of monomethyltin migration from toys by gas chromatography-mass spectrometry and confirmation of its false positive

1.
Guangdong Inspection and Quarantine Technology Center, Guangzhou 510623, China;
2.
School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510640, China

Received Date: 7 June 2018

Fund Project: Planned Project of State Key Research & Development (No. 2016YFF0203705)

Based on migration procedures using simulated gastric juice specified in the EU toy Safety Standard EN 71-3:2013/A2:2017, a method was developed for the determination of monomethyltin (MMT) migration from toys by gas chromatography-mass spectrometry (GC-MS). Further, a reliable confirmation method for judgement of a false positive for MMT obtained by GC-MS, was established. After optimizing the migration conditions, derivatization steps and chromatographic parameters, the method yielded a linear range from 0.02 to 1.0 mg/L with a correlation coefficient (R²) of 0.9992. The limits of detection and quantification of the method were 0.11 and 0.32 mg/kg, respectively. The recoveries were 86.2%-104.2% under different spiked levels (0.5, 1.0 and 1.5 μg), and the relative standard deviations were 3.1%-8.2% (n=6). MMT migration ranging from 0.44 to 0.67 mg/kg was detected in the surface coating of tin-plating (Sn-Fe alloy) toy materials, which was subsequently confirmed to be false positive. Therefore, a novel confirmative approach using methanol or acetone as the migration solvent was proposed, aiming at verifying the false positive of MMT. The results showed that the previously positive MMT detected by GC-MS could no longer be detected when treated by these migration solvents.Hence, this approach can be used to confirm false positive detected for MMT after GC-MS detection.
- gas chromatography-mass spectrometry (GC-MS),
- false positive,
- confirmation,
- monometyltin (MMT),
- migration
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1.
沈阳化工大学材料科学与工程学院沈阳 110142