前吸附技术-超高压液相色谱-串联质谱法同时测定酒中24种邻苯二甲酸酯

建立了前吸附技术-超高压液相色谱-串联质谱测定酒中24种邻苯二甲酸酯含量的方法。酒类样品经稀释、净化后采用前吸附技术排除仪器管路中的本底干扰,经超高压液相色谱-串联质谱仪进行测定。采用多反应监测模式、电喷雾电离源正离子(ESI⁺)模式进行检测,外标法定量。24种邻苯二甲酸酯在0.005~2.00 mg/L范围内线性关系良好,相关系数(r)均大于0.99,检出限(S/N=3)为0.003~0.05 mg/kg。以不含增塑剂的酒类样品作为空白样品进行加标回收率试验,各种邻苯二甲酸酯化合物的回收率为75.4%~118.2%,相对标准偏差(RSD)为4.0%~11.2%。该法不但可以有效排除管路中邻苯二甲酸酯本底的干扰,而且简单、灵敏、稳定。

Simultaneous determination of 24 phthalates in liquors using front adsorption technology and ultra performance liquid chromatography-tandem mass spectrometry

A method for the simultaneous determination of 24 phthalates in liquors was developed by using front adsorption technology and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were diluted and cleaned-up by an HLB solid phase extraction cartridge. The front adsorption technology was used to suppress the interferences which came from plastic pipes in the UPLC-MS/MS. And then the targets were analyzed by UPLC-MS/MS under the positive ion mode using multiple reaction monitoring (MRM) mode. The calibration curves showed a good linearity in the range of 0.005-2.00 mg/L with r>0.99. The limits of detections (S/N=3) were 0.003-0.05 mg/kg. The average recoveries of the spiked samples were between 75.4% and 118.2% with the relative standard deviations (RSDs) of 4.0%-11.2%. The method could be used to simultaneously confirm the multi-residue of the 24 phthalates in liquors. And the method is simple, sensitive and stable.