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目的建立膳食样品中16种邻苯二甲酸酯的同位素稀释凝胶渗透色谱净化(GPC)-气相色谱(GC)-串联质谱(MS)检测方法。方法加入同位素内标的膳食样品用正己烷饱和过的乙腈超声提取,GPC净化,DB-5 ms毛细管色谱柱分离(30 m×0.25 mm,0.25μm),GC-MS选择离子监测模式(SIM)测定,内标法定量。结果 16种邻苯二甲酸酯在8类膳食样品中的平均添加回收率为52.3%~124.7%;RSD为1.6%~16.2%;检出限为0.03~0.06 mg/kg。结论该方法简便、灵敏、准确,适用于膳食样品中邻苯二甲酸酯的检测。
Objective To establish an isotope dilution gel permeation chromatography (GPC) - gas chromatography (GC) - tandem mass spectrometry (MS) detection method for 16 kinds of phthalates in dietary samples. Methods The isotope internal standard dietary samples were extracted with acetonitrile saturated with n-hexane, purified by GPC, separated on a DB-5 ms capillary column (30 m × 0.25 mm, 0.25 μm) and analyzed by GC-MS with selected ion monitoring mode , Internal standard method. Results The average recoveries of 16 phthalates in 8 dietary samples ranged from 52.3% to 124.7%. The RSDs ranged from 1.6% to 16.2%. The limits of detection were from 0.03 to 0.06 mg / kg. Conclusion The method is simple, sensitive and accurate and is suitable for the determination of phthalates in dietary samples.