Citation: 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. doi: 10.3724/SP.J.1123.2015.06035 shu

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

LIU Hongcheng ¹ ,
LI Ning ^1,2 ,
LIN Tao ¹ ,
SHAO Jinliang ¹ ,
LI Qiwan ^1,,

1.
1. Laboratory of Quality & Safety Risk Assessment for Agro-Product (Kunming), Ministry of Agriculture, Quality Standard and Testing Technology Institute of Yunnan Academy of Agriculture Science, Kunming 650223, China;

Corresponding author: LI Qiwan,
Received Date: 23 June 2015

Fund Project: 云南省科技惠民计划重点项目(2013RA012) (2013RA012)科技创新平台建设计划项目(2014DA001). (2014DA001)

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.
- matrix solid phase dispersion (MSPD),
- ultra performance liquid chromatography (UPLC),
- mass spectrometric detector (MSD),
- estrogenic steroids,
- milk
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沈阳化工大学材料科学与工程学院沈阳 110142