%0 Journal Article %T Simultaneous determination of 7 female sex hormones in essential oil by high performance liquid chromatography- tandem mass spectrometry with isotope dilution
同位素稀释-超高效液相色谱-串联质谱法同时测定精油中的7种雌性激素 %A HUANG Baifen %A HAN Zheng %A XU Xiaomin %A CAI Zengxuan %A JIANG Wei %A REN Yiping %A
黄百芬 %A 韩铮 %A 徐小民 %A 蔡增轩 %A 姜维 %A 任一平 %J 色谱 %D 2011 %I %X 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. %K isotope dilution %K ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) %K female sex hormones %K essential oil
同位素稀释 %K 超高效液相色谱-串联质谱 %K 雌性激素 %K 精油 %U http://www.alljournals.cn/get_abstract_url.aspx?pcid=6E709DC38FA1D09A4B578DD0906875B5B44D4D294832BB8E&cid=6579068328FE643F&jid=4D81E042D77AFEC6881D14759692069C&aid=50D9FC051B35901A0A0B457861108565&yid=9377ED8094509821&vid=771469D9D58C34FF&iid=CA4FD0336C81A37A&sid=A04140E723CB732E&eid=C5154311167311FE&journal_id=1000-8713&journal_name=色谱&referenced_num=0&reference_num=15