摘要:
本研究建立了塑料玩具中48种致敏性芳香剂的气相色谱-质谱(GC/MS)同时检测方法。用四氢呋喃溶解粉碎的样品,甲醇沉淀塑料基质,离心后取上清液进行 GC/MS 检测。结果表明,金合欢醇和新铃兰醛在1~8 mg/L,反式-2-庚烯醛、香茅醇、2-辛炔酸甲酯、香叶醇、柠檬醛、对甲氧基苄醇、肉桂醇、假紫罗酮、戊基肉桂醇在0.2~8 mg/L,其余37种化合物在0.1~8 mg/L 范围内具有良好的线性关系,线性相关系数为0.9962~0.9999。在自制的3种塑料材质(ABS、PVC 和 PC)阳性样品中,致敏性芳香剂的回收率为60.5%~112.3%,相对标准偏差为3.2%~4.6%。其中在 ABS 塑料玩具中,添加浓度为5和100 mg/kg的48种致敏性芳香剂的加标回收率为83.8%~112.2%,相对标准偏差为2.9%~9.3%,检出限为0.21~13.48 mg/kg,定量限为0.71~44.94 mg/kg。本方法操作简单、提取率高、净化效果好,可用于塑料玩具中48种致敏性芳香剂的实际检测分析。
Abstract:
A method of gas chromatography-mass spectrometry (GC/MS)was devel-oped for the determination of 48 fragrance allergens in plastic toys.The analytes were dissolved from crushed samples using tetrahydrofuran.The matrix in plastic toys was precipitated by methanol,and the supernatant was injected into GC/MS after high speed centrifugation.The result shows that the linear ranges are from 1 mg/L to 8 mg/L for farnesol and hydroxy-methylpentylcyclohexenecarboxaldehyde,from 0.2 mg/L to 8 mg/L for trans-2-heptenal, citronello, methyl heptine carbonate, geraniol, citral, anisyl alcohol,cinnamyl alcohol,amylcinnamyl alcohol and 6,10-dimethyl-3,5,9-undeca-trien-2-one,from 0.1 mg/L to 8 mg/L for other 37 fragrance allergens with good corre-lation coefficients (r ≥0.996 2).The recoveries of ABS,PVC and PC plastic positive samples added fragrance allergens are 60.5%-1 12.3%,the relative standard deviations (RSDs)are 3.2%-4.6%.The recoveries of added 48 fragrance allergens to ABS plastic negative samples are 83.8%-1 12.2%.The relative standard deviations (RSDs )are 2.9%-9.3%.The limits of detection are from 0.21 mg/kg to 13.48 mg/kg,and the limits of quantification are from 0.71 mg/kg to 44.94 mg/kg.This method is simple, rapid,reliable,which is suitable for the determination of 48 fragrance allergens in plastic toys.
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