Lü Qing, Zang Qing, Bai Hua, Li Haiyu, Kang Suyuan, Wang Chao
Institute of Industrial Product Inspection, Chinese Academy of Inspection and Quarantine, Beijing 100123, China.
Se Pu. 2012 May;30(5):480-6. doi: 10.3724/sp.j.1123.2011.12005.
A method of gas chromatography-ion trap mass spectrometry (GC-IT-MS) was developed for the determination of 21 fragrance allergens in sticker toys, plush toys and plastic toys. The experimental conditions, such as sample pretreatment conditions, and the analytical conditions of GC-IT-MS, were optimized. The sticker toy samples and plush toy samples were extracted with acetone by ultrasonic wave, and the extracts were separated on an Agilent HP-1 MS column (50 m x 0.2 mm x 0.5 microm), then determined by IT-MS and quantified by external standard method. The plastic toy samples were extracted by the dissolution-precipitation approach, cleaned up with an Envi-carb solid phase extraction column and concentrated by rotary evaporation and nitrogen blowing, then determined by GC-IT-MS and quantified by external standard method. The calibration curves showed good linearity in the range of 0.002-50 mg/L with the correlation coefficients greater than 0.996 8. The limits of quantification (LOQ, S/N > 10) were 0.02-40 mg/kg. The average recoveries of the target compounds spiked in the sample at three concentration levels were in the range of 82.2%-110.8% with the relative standard deviations (RSDs) of 0.6%-10.5%. These results show that this method is accurate and sensitive for the qualitative and quantitative determination of the 21 fragrance allergens in the 3 types of toys.
建立了一种气相色谱 - 离子阱质谱法(GC - IT - MS)用于测定贴纸玩具、毛绒玩具和塑料玩具中的21种香料过敏原。对实验条件,如样品预处理条件以及GC - IT - MS的分析条件进行了优化。贴纸玩具样品和毛绒玩具样品用丙酮超声提取,提取物在安捷伦HP - 1 MS柱(50 m×0.2 mm×0.5 µm)上分离,然后通过IT - MS测定并用外标法定量。塑料玩具样品采用溶解 - 沉淀法提取,用Envi - carb固相萃取柱净化,经旋转蒸发和氮气吹干浓缩,然后通过GC - IT - MS测定并用外标法定量。校准曲线在0.002 - 50 mg/L范围内呈良好线性,相关系数大于0.996 8。定量限(LOQ,S/N > 10)为0.02 - 40 mg/kg。在三个浓度水平下加标到样品中的目标化合物的平均回收率在82.2% - 110.8%范围内,相对标准偏差(RSD)为0.6% - 10.5%。这些结果表明该方法对于三种类型玩具中21种香料过敏原的定性和定量测定准确且灵敏。