化妆品中邻苯二甲酸酯的气相色谱-质谱测定法

Determination of Dibutyl Phthalate and Bis(2-ethylhexyl) Phthalate in Cosmetics by Gas Chromatography-Mass Spectrometry

目的建立以气相色谱-质谱联用技术测定化妆品中邻苯二甲酸二丁酯(DBP)和邻苯二甲酸二(2-乙基己基)酯(DEHP)含量的方法。方法化妆品样品用甲醇或乙酸乙酯提取,采用气相色谱法进行分离,采用质谱法进行定性、定量。结果DBP的线性范围为0.5～100.0μg/ml,其标准曲线回归方程为y=2×106x-2×106,相关系数为0.9996。DEHP的线性范围为5.5～110.0μg/ml,其标准曲线回归方程为y=988223x-7×106,相关系数为0.9959。以3倍信噪比进行计算,当取样1.0g,定容至10.0ml时,样品中DBP和DEHP的检出限均为1.0mg/kg;当取样为0.2g,定容至10.0ml时,DBP和DEHP的检出限均为5.0mg/kg。DBP和DEHP回收率分别为90.8%～119.0%和90.4%～115.3%,RSD分别为4.8%～9.8%和6.0%～8.6%。结论该方法灵敏度较高,结果准确稳定,适用于化妆品中DBP和DEHP含量的检测。

Objective To develop a method for the determination of DBP and DEHP in cosmetics by GC-MS. Methods The samples was extracted by methanol or acetic ether, DBP and DEHP were separated by GC and determined by MS. Results The linear range, regression equation of calibration curve and correlation coefficient were 0.5-100.0 μg/ml, y=2×106 x-2×106, 0.999 6 for DBP respectively and 5.5-110.0 μg/ml, y=988 223 x-7×106, 0.995 9 for DEHP respectively. Based on threefold ratio of signal and noise, as the sample was 1.0 and 0.2 g respectively, the volume was 10.0 ml, the detection limits were 1.0 and 5.0 mg/kg respectively for both DBP and DEHP. The recovery rates were 90.8%-119.0% for DBP and 90.4%-115.3% for DEHP. Relative standard deviations were 4.8%-9.8% for DBP and 6.0%-8.6% for DEHP. Conclusion This method is sensitive, accurate and high reproducible, and was applicable to the determination of DBP and DEHP in the cosmetics.