Zheng Xianghua, Lin Liyi, Fang Enhua, Huang Yonghui, Zhou Shuang, Zhou Yu, Zheng Xiaoyan, Xu Dunming
Inspection and Quarantine Technology Center, Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China.
Se Pu. 2012 Jan;30(1):27-32. doi: 10.3724/sp.j.1123.2011.08019.
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.
建立并评估了一种采用固相萃取-气相色谱-质谱联用(SPE-GC-MS)同时测定食品样品中23种邻苯二甲酸酯的方法。样品用正己烷或乙腈萃取,并用玻璃ProElut PSA固相萃取柱净化。采用气相色谱-质谱联用仪在选择离子监测(SIM)模式下进行定性和定量分析。研究了不同食品的萃取过程。邻苯二甲酸酯的校准曲线在0.05-5 mg/L范围内呈良好线性(邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)为0.5-5 mg/L),相关系数(r)在0.984 8至0.999 6之间。食品样品中邻苯二甲酸酯的检测限为0.005至0.05 mg/kg(S/N = 3),定量限为0.02至0.2 mg/kg(S/N = 10)。在10种食品基质中添加23种分析物的平均回收率为77%至112%,相对标准偏差(RSD,n = 6)为4.1%-12.5%。该方法操作简便、准确度和精密度高,适用于同时测定食品中的23种邻苯二甲酸酯。