GC-MS/MS法测定蔬菜中16种邻苯二甲酸酯

Determination of 16 phthalic acid esters in vegetables by GC-MS /MS

目的建立同时检测蔬菜中16种邻苯二甲酸酯(PAEs)的气相色谱-串联质谱(GC-MS/MS)分析方法。方法样品用乙腈提取并旋蒸后经玻璃Florisil柱净化,采用DB-5MS色谱柱程序升温分离,选择多反应监测模式(MRM)测定。结果在本试验条件下,16种PAEs分离较好,该法检出限为0.05μg/L^0.3μg/L,定量限为0.15μg/L^0.9μg/L,检测质量浓度线性范围为0.02μg/L^2.0μg/L,相关系数均>0.994,16种PAEs的加标回收率为92.1%~112.5%,相对标准偏差为1.8%~6.7%。结论该法操作简单、可靠,可用于蔬菜中多种PAEs的确证与定量检测。

Objective To establish gas chromatography - mass spectrometry/mass spectrometry（ GC - MS/MS） for detection of 16 phthalic acid esters（PAEs） in vegetables. Methods The PAEs in samples were extracted with acetonitrile, and then cleaned - up by using glass Florisil SPE after rotary evaporation, and finally separated on a DB - 5MS column with temperature programming, and detected quantitatively in multiple reaction monitoring mode （MRM）. Results 16 phthalic acid esters could be completely separated under the condition of GC - MS/MS. The detection limits of this method were 0.05 μg/L - 0.3 μg/L, the limits of quantittation were 0.15 p.g/L - 0.9 μg/L, the linear ranges were 0.02 μg/L - 2.0 p,g/L, the relative coefficient was more than 0. 994, the recovery of the method were 92.1% -112.5%, the relative standard deviations were 1.8% 6.7%. Conclusion The method is simple, reliable and it can be applied to detection and confirmation of phthalic acid esters in vegetables.