Simultaneous determination of sex hormones in egg products by ZnCl2 depositing lipid, solid-phase extraction and ultra performance liquid chromatography/electrospray ionization tandem mass spectrometry.
A method was developed for simultaneous determination of residues of 17 sex hormones in egg products. Target compounds were extracted from samples with methanol in an ultrasonic bath, effectively separated from lipids in the extracts by ZnCl(2) depositing filtration and purified using a C(18) solid-phase extraction (SPE) and followed by NH(2) SPE cartridge. The analytes were quantified by liquid chromatography using a BEH C(18) column coupled to an electrospray ionization tandem mass spectrometer (LC-ESI-MS/MS) operating in negative mode for estrogens and in positive multiple reaction monitoring mode for androgens. The parameters of the mass spectrometer and the composition of mobile phase and additives were also optimized to enhance detection sensitivity. Average recoveries of the target compounds varied from 70.0% to 121.0% with relative standard deviations ranging from 2.3% to 11.2% at two fortification levels. The limits of detection (LOD) of the method were from 0.002 μg kg(-1) to 0.23 μg kg(-1) and the limits of quantification (LOQ) were in the range of 0.007-0.76 μg kg(-1).
Wang
Quan-lin
QL
Ningbo Academy of Product Quality Supervision & Inspection, No. 28 Wangai Road, Jiangdong, Zhejiang, Ningbo 315041, China. quanlinwang@163.com
Zhang
Ai-zhi
AZ
Pan
Xu
X
Chen
Li-ren
LR
D002712:Chlorides / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004531:Eggs / Q000032:analysis*; D005504:Food Analysis; D012739:Gonadal Steroid Hormones / Q000032:analysis* / Q000302:isolation & purification; D052616:Solid Phase Extraction / Q000379:methods*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D017967:Zinc Compounds / Q000737:chemistry*
D002712:Chlorides; D012739:Gonadal Steroid Hormones; D017967:Zinc Compounds; C016837:zinc chloride