Objective To develop a detection method with ultra-high performance liquid chromatogra-phy-high resolution mass spectrometry(UPLC-HRMS) for fast screening of doping substances in pastes,so as to strengthen the drug-borne doping risk prevention system.Methods The paste samples were removed the covering film and extracted by using tert-butyl methyl ether and anhydrous ethanol,respectively.The extracts were combined and blown dry under nitrogen flow at 40 ℃,and methanol was used to dissolve the residues,which were then filtered and analyzed with the Thermo Vaniquish-Q Exactive Plus.Then,3 μL of the solution was injected into and separated by the Agilent ZORBAX-Eclipse C18 column (2.1 × 100 mm,1.8 μm),and the gradient elution was performed with 10 mM ammonium formate (containing 0.1％ formic acid,pH3.5) and acetonitrile as mobile phase.The 170 kinds of doping substances were detected in positive ion electrospray (ESI+) and negative ion electro-spray(ESI-) respectively under Full Mass/data-dependent mass spectrometry(Full MS/ddMS2) mode.Re-sults The results showed that the method had good selectivity and samples were stable within 48 h af-ter pretreatment.The detection limit(LOD) of 92 doping substances were about 3 ng/g,while that of another 31 and 47 ones was about 6 ng/g and 30 ng/g,respectively.In this study,among 10 paste samples,4 were tested positive for strychnine,and 3 were positive for higenamine and ephedrine,re-spectively.Conclusion A fast screening method for 170 kinds of doping substances in 9 categories is developed by using ultra-high performance liquid chromatography with high resolution mass spectrome-try in this study.Such method proves to be simple,sensitive and reliable,which is suitable for fast screening of doping substances in pastes.

Objective To develop a detection method with ultra-high performance liquid chromatogra-phy-high resolution mass spectrometry(UPLC-HRMS) for fast screening of doping substances in pastes,so as to strengthen the drug-borne doping risk prevention system.Methods The paste samples were removed the covering film and extracted by using tert-butyl methyl ether and anhydrous ethanol,respectively.The extracts were combined and blown dry under nitrogen flow at 40 ℃,and methanol was used to dissolve the residues,which were then filtered and analyzed with the Thermo Vaniquish-Q Exactive Plus.Then,3 μL of the solution was injected into and separated by the Agilent ZORBAX-Eclipse C18 column (2.1 × 100 mm,1.8 μm),and the gradient elution was performed with 10 mM ammonium formate (containing 0.1％ formic acid,pH3.5) and acetonitrile as mobile phase.The 170 kinds of doping substances were detected in positive ion electrospray (ESI+) and negative ion electro-spray(ESI-) respectively under Full Mass/data-dependent mass spectrometry(Full MS/ddMS2) mode.Re-sults The results showed that the method had good selectivity and samples were stable within 48 h af-ter pretreatment.The detection limit(LOD) of 92 doping substances were about 3 ng/g,while that of another 31 and 47 ones was about 6 ng/g and 30 ng/g,respectively.In this study,among 10 paste samples,4 were tested positive for strychnine,and 3 were positive for higenamine and ephedrine,re-spectively.Conclusion A fast screening method for 170 kinds of doping substances in 9 categories is developed by using ultra-high performance liquid chromatography with high resolution mass spectrome-try in this study.Such method proves to be simple,sensitive and reliable,which is suitable for fast screening of doping substances in pastes.

Objecave To develop a sensitive and specific LC-MS/MS method for determination of testolactone in human urine.Methods A C_(18 )column(2.1×50mm,3.5μm) was used.The mobile phase Was a mixture of acetonitrile and the buffer solution(ammonium acetate-water solution adjusted with formic acid to pH 3.5)at a flow rate of 0.5ml/min.A mass spectrometer equipped with electrospray ionization source was used as a detector and operated in the positive mode.In multiple reaction monitoring(MRM)mode,the ion transitions of m/z 301→121 and m/z 301→25 was used to qualify and quantify the testolactone,respectively.Results Chromatograms showed no endogenous interfering peaks with the urine blank sample.Each analysis was completed within 7min The calibration wag linear in the concentration range within 0.1～50μg/ml.The intra-batch and inter-batch RSD were less than 10%.The recovery rate of the extraction was about 60%.Conclusions The method is proved to meet the requirements of WADA and be suitable for routine screening.

A method has been developed for the determination of stimulants in products of nutritional supplement. The stimulants in the samples were extracted with a solution of sodium hydroxide and then cleaned up by liquid -liquid partitioning.The extracted stimulants were analyzed by gas chromatography with HP-5capilary column and detected by the Nitrogen-Phosphorus detector (NPD). The results showed that the method had good purifying effect with high sensitivity. The operation was also simple and quick. The detection limit ranged from 5 to 40 ?g/L and the average recovery rate was 75.4%～143.1% with relative standard deviations (RSDs) ranged from 0.27% to 5.5%.

To study the chemical constituents of Buddleja lindleyana Fort.. Methods　The constituents were isolated and purified by various chromatographic methods and structurally identifed by physico-chemical properties and spectral analysis. Results　10 compounds were obtained as α-spinasterol (Ⅰ), stigmasterol (Ⅱ)， β-sitosterol (Ⅲ), ursolic acid (Ⅳ), oleanolic acid (Ⅴ),phenanthrene (Ⅵ), glycerol mono tetracosanoate (Ⅶ), nonacosane (Ⅷ), acaciin (Ⅸ) and 6-O-vanilloyl-ajugol (Ⅹ). Conclusion　All these compounds were obtained from this plant for the first time.