Determination of nine estrogenic steroids in milk using matrix solid phase dispersion-ultra performance liquid chromatography with mass spectrometric detector

doi:10.3724/SP.J.1123.2015.06035

Abstract

Abstract:

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 μ g/kg. The limits of quantification (LOQ) were 2-20 μ g/kg.

Key words: estrogenic steroids, mass spectrometric detector (MSD), matrix solid phase dispersion (MSPD), milk, ultra performance liquid chromatography (UPLC)

CLC Number:

O658

LIU Hongcheng, LI Ning, LIN Tao, SHAO Jinliang, LI Qiwan. Determination of nine estrogenic steroids in milk using matrix solid phase dispersion-ultra performance liquid chromatography with mass spectrometric detector[J]. Chinese Journal of Chromatography, 2015, 33(11): 1163-1168.

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