固相萃取–气相色谱–串联质谱法检测土壤中15种邻苯二甲酸酯

建立了固相萃取结合气相色谱串联质谱联用仪检测土壤中15种邻苯二甲酸酯残留的方法。样品采用丙酮和石油醚超声提取,取上清液浓缩,上弗罗里硅土固相萃取柱净化,收集洗脱液,定容,以气相色谱串联质谱法分析。该方法在20~2 000 ng/g范围内线性关系良好(r~20.999 0),检出限(S/N=3)为0.12~0.61 ng/g。20,50,200 ng/g 3个添加浓度的15种邻苯二甲酸酯的加标回收率在78.9%~101.8%之间,测定结果的相对标准偏差为0.19%~8.34%(n=5)。该方法准确、灵敏,符合痕量分析的要求,适用于土壤中邻苯二甲酸酯类残留的分析。

Determination of 15 Kinds of Phthalate Esters in Soil by Using Solid Phase Extraction-Gas Chromatography-Tandem Mass Spectrometry

A method for the determination of 15 phthalate esters in soil by solid phase extraction and gas chromatogra-phy tandem mass spectrometry was developed. The samples were extracted with acetone and petroleum ether.The supernatant was concentrated and cleaned up on a Florisil solid phase extraction column. The eluent was collected and then analyzed by gas chromatography tandem mass spectrometry. The calibration curve was linear in the range of 20-2000 ng/g (r2> 0.9990) and the detection limits (S/N =3) were 0.12-0.61 ng/g. The recoveries of 15 phthalates at 20, 50 and 200 ng/g ranged from 78.9% to 101.8% with RSDs of 0.19%-8.34%(n=5). The method is accurate,sensitive and suitable for the analysis of phthalic acid esters in soil.