A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 s...A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L^(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg^(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg^(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues.展开更多
The "solidified liquid layer" model has been examined using a quartz crystal microbalance(QCM) with a polymeric matrix.The model is shown to give a reasonable explanation for the following experimental obser...The "solidified liquid layer" model has been examined using a quartz crystal microbalance(QCM) with a polymeric matrix.The model is shown to give a reasonable explanation for the following experimental observations:(i) The opposite response of the QCM and surface plasmon resonance(SPR) for the activation process;(ii) the marked difference in the responses for IgG/anti-IgG interaction between QCM and SPR.Theoretical analysis and experimental results indicated that QCM is sensitive to the thickness change of the "solidified liquid layer" but not the mass of captured biomolecules(i.e.,the immobilized mass),implying caution must be taken in interpreting QCM results.展开更多
基金supported by the Natural Science Foundation of Zhejiang Province,China(No.LY17C200009)the Foundation of Zhejiang Educational Committee(No.Y201328477)
文摘A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L^(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg^(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg^(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues.
基金supported by the 100 Talents Programme of Chinese Academy of Sciences(08BM031001)the Fok Ying Tung Education Foundation (114013) to H.M.the National Basic Research Program of China (2009CB320300)
文摘The "solidified liquid layer" model has been examined using a quartz crystal microbalance(QCM) with a polymeric matrix.The model is shown to give a reasonable explanation for the following experimental observations:(i) The opposite response of the QCM and surface plasmon resonance(SPR) for the activation process;(ii) the marked difference in the responses for IgG/anti-IgG interaction between QCM and SPR.Theoretical analysis and experimental results indicated that QCM is sensitive to the thickness change of the "solidified liquid layer" but not the mass of captured biomolecules(i.e.,the immobilized mass),implying caution must be taken in interpreting QCM results.
