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色谱 2011
Simultaneous determination of 7 female sex hormones in essential oil by high performance liquid chromatography- tandem mass spectrometry with isotope dilution
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Abstract:
A reliable ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of 7 female sex hormones (estriol, estradiol, estrone, ethinyloestradiol, dienestrol, hexestrol, diethylstilbestrol) in essential oil was developed. The sample was extracted by ethylacetate-normal hexane solution (2:98, v/v) and the extract was purified by a silica solid phase extraction-based clean-up column. Then, the analytes were separated on an ACQUITY UPLC BEH SHELD RP18 column (100 mm×2.1 mm, 1.7 μm) in gradient elution with the mobile phases of water and acetonitrile. The separated compounds were detected with a Waters Xevo TQ MS tandem quadrupole mass spectrometer operated in negative electro-spray ionization using multiple reaction monitoring mode. Estriol-D3, estradiol-D3 and diethylstilbestrol-D6 were used as the internal standards to reduce the matrix effects. The limits of detection and quantitation for the 7 female sex hormones in essential oil were 0.3~7 μg/kg and 1~20 μg/kg, respectively. Good linear relationships and high correlation coefficients (r2≥0.997) were obtained in the mass concentration range of 20~500 μg/L. The average recoveries were 88.5%~114.8% and the intra-assay relative standard deviations were 4.8%~18.9% at the spiked levels of 20~500 μg/kg. Finally, a total of 12 samples randomly collected from different supermarkets in Zhejiang Province were screened for the 7 female sex hormones by the proposed method. The results showed that only one sample contained estradiol and estrone.
