洗发水和沐浴液中1,4-二噁烷含量测定溶剂的选择研究

Study on selectivity of solvent for determination of 1,4-dioxane in shampoo and bath lotion

采用了顶空-GC-MS测定化妆品中的二噁烷。比较了不同质量分数的5种盐溶液:碳酸钾、氯化钠、硫酸钠、硫酸铵和硫酸镁溶液作为溶剂对二噁烷产生的盐析效果。实验结果表明,碳酸钾溶液有利于提高二噁烷在顶空瓶中的浓度,具有较好的盐析效果。同时,比较了不同质量分数和体积的碳酸钾溶液对顶空瓶中二噁烷浓度的影响,确定样品处理方法为:顶空瓶中加入2 g待测样品和3 g碳酸钾固体,用水稀释定容至10 mL。该方法对检测二噁烷含量具有较高的准确度,回收率为97.6%～110.5%,相对标准偏差为3.75%～9.34%,检出限为1.0 mg/kg。

Determination with headspace-gas-chromatography-mass spectrometry for dioxane in shampoo and bath lotion is developed. Potassium carbonate, sodium chloride, sodium sulfate, ammonia sulfate and bitter salt solutions are compared as solvents to produce salting-out. The results indicate that potassium carbonate solution increases the concentration of dioxane in headspace bottles. Comparing the effect of different mass fractions and volumes of potassium carbonate solution on dioxane in headspace bottles ,the pretreatment measure of samples is selected ：2 g of sample and 3 g of potassium carbonate with water to 10 mL in headspace bottle. The recovery rates of dioxane are 97.6% - 110. 5%. The RSDs of dioxane are 3.75% -9. 34%. The low detection limit of the method is 1.0 mg/kg.