A headspace/gas chromatography - tandem mass spectrometric ( HS/GC -MS/MS) method was established for the determination of 1, 4-dioxane residues in synthetic detergents and cosmetics. The samples were mixed with water, then sodium chloride was added to produce the " salting -out" effect. After oscillation, 1, 4-dioxane in sample was dissolved completely. The sample mixed with water was oscillated for 30 min at 80℃ to get gas - liquid balance state and then the upper clear gas was prepared. The detection was carried out by GC - MS/MS under the multiple-reaction monitoring (MRM) mode. Good linearity in the concentration range of 0. 1 - 100 mg/L was obtained, with a correlation coefficient of 0. 999 8. The limit of detection ( LOD) was 0. 010 mg/kg and the limit of quantitation ( LOQ) was 0. 035 mg/kg. The average recoveries were in the range of 98% - 103% , with relative standard deviations( RSDs) of 0. 44% -2. 1% . The accuracy, reliability and sensitivity of the method made it suitable for the determination of 1, 4-dioxane in synthetic detergents and cosmetics.%建立了顶空/气相色谱-串联质谱(HS/GC-MS/MS)测定合成洗涤剂和化妆品中二(口恶)烷含量的分析方法.将样品与适量的水混溶,加入固体氯化钠产生“盐析”效应后再通过超声振荡,使样品中的二(口恶)烷充分溶解.此后将样品瓶于80℃混合摇振30 min达到气液平衡,顶空进样,在GC-MS/MS多反应监测模式(MRM)下测定,二(口恶)烷在质量浓度0.1～100 mg/L范围内呈良好线性,相关系数为0.9998,检出限(S/N=3)为0.010 mg/kg,定量下限(S/N=10)为0.035 mg/kg,平均加标回收率为98％～103％,相对标准偏差为0.44％～2.1％.该方法能有效消除复杂基质的干扰,结果准确可靠,灵敏度高,重现性好,适用于合成洗涤剂和化妆品中痕量二(口恶)烷的测定.
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