An analytical method for the multiresidue determination of nine estrogenic steroids in milk was developed by modified matrix solid phase dispersion (MSPD) purification and ultra performance liquid chromatography (UPLC) with mass spectrometric detector (MSD). The sensitivity and accuracy of MSD were better than that of ultraviolet detector. In comparison with traditional mass spectrometry, the merits of MSD were simpler in operation and shorter in starting time (5 min). The results showed that the limits of detection of the compounds with nucleophilic substitution were high in positive ion mode of MSD and were easily affected by environmental conditions. The matrix effects of milk samples reduced from 84%-160% to 80%-121% after MSPD purification. The intraday precision and interday precision of the nine estrogenic steroids were 0.87%-1.78% and 1.82%-3.79%, respectively. The average recoveries were 68.7%-94.7%, and the relative standard deviations (RSDs) were less than 10%. The limits of detection (LODs) were 0.5-10 mu g/kg. The limits of quantification (LOQ) were 2-20 mu g/kg.
[1]Yunnan Acad Agr Sci, Qual Stand & Testing Technol Inst, Minist Agr, Lab Qual & Safety Risk Assessment Agroprod Kunmin, Kunming 650223, Yunnan, Peoples R China.
[2]Kunming Med Univ, Dept Pharmaceut Sci, Kunming 650500, Yunnan, Peoples R China.
(8.0+极速模式)