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目的建立了气相色谱-质谱测定乳和霜类化妆品中21种塑化剂含量的测定方法。方法采用PAE净化小柱对样品进行净化处理。采用甲基(5%苯基)聚硅氧烷为固定相的DB-5MS毛细管色谱柱(30 m×250 mm,0.25μm)进行气相分离,柱温:60℃保持1 min,以20℃/min升至220℃,保持1 min,再以5℃/min升至280℃,保持4 min,总运行时间26 min;进样口温度:250℃;传输线温度:280℃;氮气流速:采用恒流模式,流速:1.0 ml/min;选取3种邻苯二甲酸酯类化合物的同位素作为内标,进行测定。结果 21种塑化剂的线性范围为0.01μg/ml~10μg/ml,r>0.999;检测限为0.02 mg/kg~0.32 mg/kg,平均加样回收率(n=9)范围为96.7%~102.5%,RSD为1.0%~5.7%。结论该方法灵敏度高、专属性好、操作简便、重现性好,可用于化妆品中塑化剂的测定。
Objective To establish a method for the determination of 21 plasticizers in milk and cream cosmetics by gas chromatography-mass spectrometry. Methods The PAE column was used to purify the sample. Gas phase separation was carried out on a DB-5MS capillary column (30 m × 250 mm, 0.25 μm) using methyl (5% phenyl) polysiloxane as the stationary phase. The column temperature was maintained at 60 ° C for 1 min and at 20 ° C / min to 220 ° C for 1 min and then to 280 ° C at 5 ° C / min for 4 min with a total run time of 26 min; inlet temperature: 250 ° C; transfer line temperature: 280 ° C; nitrogen flow rate: Flow rate, flow rate: 1.0 ml / min; the isotopes of three kinds of phthalate compounds were selected as the internal standard, and the determination was carried out. Results The linear range of the 21 plasticizers was 0.01 μg / ml ~ 10 μg / ml with r> 0.999. The detection limit was 0.02 mg / kg ~ 0.32 mg / kg, and the average recovery ranged from 96.7% ~ 102.5%, RSD was 1.0% ~ 5.7%. Conclusion The method has high sensitivity, specificity, easy operation and good reproducibility. It can be used in the determination of plasticizers in cosmetics.