气相色谱-质谱测定化妆品中21种塑化剂的含量

Determination of phthalate acid esters in cosmetic by GC-MS

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 A gas chromatography mass spectrometry（GC-MS） was developed for the determination of 21 phthalate acid esters in milk and cream of cosmetic.Methods After being extracted by n-hexane purified by PAE column,21 phthalate acid esters were separated from gas phase with DB-5MS capillary chromatographic column（30 m × 250 mm,0.25 m） with methyl（5% phenyl polysiloxane） the stationary phase stationary phase,and column temperature was 60 ℃ then increased to 220 ℃ at 20 ℃ per minute.Column temperature was maintained at 220 ℃ for 1 minutes,then increased to 280 ℃at 5 ℃ per minute,column temperature was maintained at 280 ℃ for 4 minutes,the total run time is 26 minutes,injector temperature was set at 250 ℃ and transmission line at 280 ℃ respectively.The gas flow rate was 1.0 ml/min.Results Calibration curves of 21 phthalate acid esters were Linear in the ranges of 0.01 μg/ml - 10 μg/ml,the detection limit ranged in0.02 mg/kg - 0.32 mg/kg for 21 phthalate acid esters.The average recovery were 96.7% - 102.5%（n = 9） RSD 1.0% -5.7%.Conclusion The method is simple,sensitive,accurate,specific and reproducible.