| PART 1:DETERMINATION AND RESEARCH OF SEVENTEEN DISPERSE DYES IN TEXTILETextile is closely related to human life, the improper using of allergenic and prohibited disperse dyes is bound to affect the body health. In this paper, ultra-high performance convergence chromatograph coupled with triple quadrupole tandem mass spectrometry (UPC2-TQMS) method was used to detect and analyse the 17 kinds of disperse dyes in textile as follows:1. Establish a highly sensitive and fast procedure for the control of 17 allergenic and prohibited disperse dyes including disperse yellow 1, disperse blue 1, disperse orange 3, disperse red 11, disperse yellow 3, disperse yellow 9, disperse yellow 39, disperse blue 3, disperse red 1, disperse orange 1, disperse blue 106, disperse red 17, disperse blue 102, disperse yellow 49, disperse blue 124, disperse orange 37 and disperse brown 1 by UPC2-TQMS. Stationary phases, backpressure and column temperature were investigated. All 17 disperse dyes were simultaneously separated in 5min. The dyes were monitored via multiple reaction monitoring (MRM). The LOQ and LOD ranges of dyes were 0.1～2.0 μg·mL-1 and 0.02～1.0 μg·mL-1, respectively. The calibrations were performed and good linear relationship (R>0.99). Satisfactory recoveries were 70.55～103.03%. The method was applied to some textile samples.2. Four stationary phases, BEH, BEH 2-ethyl-pyridine, HSS C18 SB and CSH fluorophenyl were investigated about the separation condition to the disperse dyes that contain anthraquinone, hydroxyl and amino groups. The results show that HSS C18 SB phase presents a significantly polar characteristic which lead to overall retention time extension. On the CSH Fluorophenyl, dyes contain the structure of the anthraquinone have strong interaction with this column. The experiment also found that CSH Fluorophenyl has good selectivity and separation to the sample containing aromatic structure cis-trans isomers.PART 2:METABOLOMICS PROFILES PREDICT SURVIVAL OF PATIENTS WITH ADVANCED LUNG ADENOCARCINOMA TREATED WITH GEFITINIBGefitinib is one of the main drug for treating lung cancer, but it doesn’t have efficacy to all lung cancer patients. How to determine whether Gefitinib is suitable for a patient with lung cancer is an important clinical research.In this study, metabolomics was used to analyze lung cancer serum samples from 134 patients which have different survival time by ultra-high performance liquid chromatography-time of flight mass spectrometry (UHPLC-QTOFMS). The experiment main contents and results are as follows:1. UHPLC-QTOFMS procedure for detection of 134 samples was established. We optimized the serum pretreatment method and the optimal conditions of instruments. Through Waters ACQUITY UHPLCTM BEH C18(1.7μm,2.1×100 mm I.D.) column separation, column temperature was 45℃, mobile phase was using methanol (A)-0.2% formic acid aqueous solution (B) under the flow rate 0.35 mL·min-1, sample elution time was 22 min.134 serum samples were monitored via ESI source of positive and negative mode. Eventually we acquired the metabolic fingerprint of each samples.2. The raw data of 134 samples were imported to the MarkerLynx V4.1 for peak alignment to obtain a peak list containing the retention time, m/z, and peak area of each sample. Then SIMCA-P software to carry on PLS-DA analysis, through the Kaplan Meier analyse and Log rank test. COX regression model was used to analyse multiple factors. We found out 22 major potential metabolites and further filtered 2 important biomarkers.3. The structure of the biomarkers was elucidated following an integrated method. The retention time, accurate m/z of the MS fragments and relationship in the MS/MS spectrum were studied. Then the database, HMDB was searched for matching structures. Finally we identified two phospholipid compounds as potential biomarkers. The biomakers can be applied in determining lung cancer patients whether they are suitable for taking Gefitinib.
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