title: [Simultaneous determination of 7 female sex hormones in essential oil by high performance liquid chromatography-tandem mass spectrometry with isotope dilution].
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 x 2.1 mm, 1.7 microm) 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 microg/kg and 1-20 microg/kg, respectively. Good linear relationships and high correlation coefficients (r2 > or = 0.997) were obtained in the mass concentration range of 20-500 microg/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 microg/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.
authors.affiliation: Zhejiang Provincial Center for Disease Prevention and Control, Hangzhou 310051, China.
authors.forename: Baifen
authors.initials: B
authors.lastname: Huang
authors.forename: Zheng
authors.initials: Z
authors.lastname: Han
authors.forename: Xiaomin
authors.initials: X
authors.lastname: Xu
authors.forename: Zengxuan
authors.initials: Z
authors.lastname: Cai
authors.forename: Wei
authors.initials: W
authors.lastname: Jiang
authors.forename: Yiping
authors.initials: Y
authors.lastname: Ren
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D045166:Estradiol Congeners / Q000032:analysis*; D009822:Oils, Volatile / Q000737:chemistry*; D045167:Progesterone Congeners / Q000032:analysis*; D011865:Radioisotope Dilution Technique; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D045166:Estradiol Congeners; D009822:Oils, Volatile; D045167:Progesterone Congeners