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建立了橡胶玩具中N-亚硝胺和N-亚硝胺前体物的迁移量的高效液相色谱-串联质谱(HPLC-MS-MS)的检测方法。样品经甲醇提取,采用ZORBAX Eclipse Plus C18柱,以甲酸-乙腈为流动相,梯度洗脱分离后,串联四极杆质谱多反应监测方式检测。以保留时间和子离子比定性,外标法定量。在优化条件下,该方法12 min即可完成6种待测物分析。各分析物在0.01~10 mg/L范围内线性关系良好,相关系数均大于0.999。方法检出限为0.001 mg/L,低于欧盟2009/48/EC的限量要求。分析物在3个不同水平的加标回收率为79%~96%,RSD<8.2%。方法适用于橡胶玩具中N-亚硝胺类物质的快速确认和定量检测。
A method for the determination of the migration of N-nitrosamine and N-nitrosamine precursors in rubber toys by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) was established. The samples were extracted with methanol and analyzed by a ZORBAX Eclipse Plus C18 column with formic acid-acetonitrile as the mobile phase. The mobile phases were separated by gradient elution and detected by tandem quadrupole mass spectrometry. To retain the time and ion ratio qualitative, external standard method. Under optimized conditions, the method can complete 6 kinds of analytes under 12 min. The linearity of each analyte in the range of 0.01-10 mg / L was good with the correlation coefficients greater than 0.999. The limit of detection was 0.001 mg / L, which was lower than the limit of EU 2009/48 / EC. The spiked recoveries of analyte at three different levels ranged from 79% to 96% with RSD <8.2%. The method is suitable for the rapid confirmation and quantitative detection of N-nitrosamines in rubber toys.