固相萃取-气相色谱-质谱法测定食品中23种邻苯二甲酸酯

Determination of 23 phthalate esters in food by solid-phase extraction coupled with gas chromatography-mass spectrometry

建立了同时检测食品中23种邻苯二甲酸酯类化合物的固相萃取-气相色谱-质谱(GC-MS)分析方法。样品经正己烷或乙腈提取、玻璃ProElut PSA固相萃取柱净化,GC-MS选择离子监测模式(SIM)测定。考察了不同种类食品的提取、净化方法。23种邻苯二甲酸酯的线性范围除邻苯二甲酸二异壬酯(DINP)和邻苯二甲酸二异癸酯(DIDP)为0.5～5 mg/L外,其余均为0.05～5 mg/L,相关系数(r)除DIDP外均大于0.99。方法的检出限(信噪比为3)为0.005～0.05 mg/kg,定量限(信噪比为10)为0.02～0.2 mg/kg。在10种食品基质中3个加标水平的平均回收率为77%～112%,相对标准偏差(RSD,n=6)为4.1%～12.5%。该方法稳定、可靠,操作简单,适用于食品中邻苯二甲酸酯类化合物的检测与确证。

A method for the simultaneous determination of 23 phthalate esters in food samples by solid-phase extraction coupled with gas chromatography-mass spectrometry(SPE-GC-MS) was developed and evaluated.The samples were extracted with hexane or acetonitrile,and cleaned up with a glass ProElut PSA SPE column.The identification and quantification were performed by GC-MS in selected ion monitoring(SIM) mode.The extraction processes of different foods were investigated.The calibration curves of phthalate esters showed good linearity in the range of 0.05-5 mg/L(0.5-5 mg/L for diisononyl phthalate(DINP),diisodecyl-phthalate(DIDP)) with the correlation coefficients(r) between 0.9848 and 0.9996.The limits of detection of phthalate esters in food samples ranged from 0.005 to 0.05 mg/kg(S/N=3) and the limits of quantification ranged from 0.02 to 0.2 mg/kg(S/N=10).The average recoveries of 23 analytes spiked in 10 kinds of food matrices ranged from 77% to 112% with the relative standard deviations(RSDs,n=6) of 4.1%-12.5%.The method is suitable for the determination of 23 phthalate esters simultaneously in foodstuffs with easy operation,high accuracy and precision.