Simultaneous determination of six estrogens in dai products by high performance liquid chromatography-triple quadrupole-ion trap mass spectrometry coupled with matrix solid-phase dispersion and solid phase extraction

被引:4
作者
Han Shuying [1 ]
Yu Huimin [1 ]
Song Yilin [1 ]
Deng Haishan [1 ]
Chai Chuan [1 ]
Chi Yumei [1 ]
机构
[1] Nanjing Univ Chinese Med, Coll Pharm, Nanjing 210023, Jiangsu, Peoples R China
基金
中国国家自然科学基金;
关键词
high performance liquid chromatography-triple quadrupole-ion trap mass spectrometry (HPLC-Q-TRAP-MS); matrix solid-phase dispersion (MSPD); solid-phase extraction (SPE); estrogen; milk powder; liquid milk;
D O I
10.3724/SP.J.1123.2017.11043
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
Matrix solid-phase dispersion (MSPD) and solid-phase extraction (SPE) were respectively developed for the pretreatment six estrogens in milk powder and liquid milk. It was implied that MSPD was suitable for the treatment of milk powder, while SPE was suitable for liquid milk treatment. Based on the optimized pretreatment procedures, the method for the simultaneous determination of the six estrogens in different dairy products was established by high performance liquid chromatography-triple quadrupole-ion trap mass spectrometry ( HPLC-Q-TRAP-MS) . The proposed method provided low limits of detection ( LODs , 0. 01-0.05 mg/L) and limits of quantification (LOQs , 0.05 -0. 10 mg/L) , wide linearity range of 0.1-200 mg/L ( except for estriol of 0. 1 -20 mg/L) with excellent correlation coefficients (R-2) > 0.99. The average recoveries of the six estrogens in milk powder pretreated by MSPD ranged from 71.8% to 106. 0% with RSD of 1. 6% 9. 2% (n = 3) , while the corresponding average recoveries in liquid milk pretreated by SPE ranged from 70.3% to 108.4% with RSD of 2.0% and 11.0% (n=3) with spiking levels of 1.0, 5.0, and 10 mg/kg, respectively. This sensitive and reliable method meets the demand for the analysis of trace estrogen residues in complex matrices.
引用
收藏
页码:285 / 291
页数:7
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