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。
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.
参考文献
| [1] | Peng XJ.;Li YH.;Luan ZK.;Di ZC.;Wang HY.;Tian BH.;Jia ZP..Adsorption of 1,2-dichlorobenzene from water to carbon nanotubes[J].Chemical Physics Letters,20031/2(1/2):154-158. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%