摘要

In this study, a simple, rapid and accurate quantitative method for the determination of phthalate esters in infant milk powder and dairy products by GC-MS using 16 internal standards has been developed. Samples were extracted with acetonitrile and purified using PAE solid-phase extraction (SPE), the eluant was then dried with N-2 flow at 45 A degrees C and diluted with n-hexane for testing by GC-MS. The standard calibration curves were linear for all matrixes analysed, and the correlation coefficients ranged from 0.9955 to 0.9999. The LODs and LOQs were in the ranges of 1.0-100.0 A mu g kg(-1) and 3.0-300.0 A mu g kg(-1), respectively. The accuracy of this method was evaluated by measuring the recovery from spiked samples. The recoveries of all phthalates from samples spiked at three different concentrations (100.0, 500.0, and 1000.0 A mu g kg(-1)) were determined. The recovery ranges in low, intermediate and high spiked levels were 73.8-114.5 %, 76.1-102.2 % and 81.1-113.5 %, respectively, and the relative standard deviation (RSD) range of recovery results (n = 6) was 0.5-19.1 %, 0.3-6.4 % and 0.2-19.2 % at low, intermediate and high spiked levels. Furthermore, the differences in recovery and RSD were discussed when different quantitative methods were used. In addition, the matrix effect was discussed in the article.

  • 出版日期2016-7
  • 单位杭州市疾病预防控制中心