Development Of Measurement And Metrology Technology For Multiple Food Additives In Complicated Matrix

The problems of frauding and counterfeiting alcoholic products have caused widespread concern in society. Some enterprise illegally added synthetic pigment into the wine, in order to cover the defect of wine and sell seconds at best quality price. Therefore, the State Council put forward a special work for 16 kinds of important products, "To crack down on fake and shoddy manufacturing, to crack down on piracy of intellectual property" The research on trace food additives residual analysis is relatively little in liquid chromatography tandem technology. Which have significance and value of scientific research to carry out exploration and studying in the field. In this thesis, complex matrix was alcoholic liquors, including red wine and spirits. The research aim was to establish metrological technology of a variety of food additives residues in alcoholic liquors.1) A simple and highly sensitive method for the simultaneous determination of eight water-soluble food additive residues, including acesulfame potassium (ACS-K), sodium cyclamate (CYC), sodium saccharin (SAC), tartrazine (E102), amaranthus red (E123), ponceau 4R (E124), sunset yellow (E110) and brilliant blue (E133), in red wine has been developed using ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). These compounds were separated within 6 min using a BEH C18 column with a linear gradient elution program and the mobile phase of 10 mmol/L ammonium acetate solution and methanol-acetonitrile (v/v,9:1) mixed organic solvent, in which contained 0.002% trifluoroacetic acid (TFA).2) The optimized method, based on MS/MS in multiple reaction monitoring mode, gave good linearity in the test range of (0.05-300) ?g/L with correlation coefficients (?2) better than 0.9968. The limits of detection (S/N=3) for the target compounds were 0.01 ?g/L (E133),0.03?g/L (ACS-K),0.01?g/L (CYC),0.2?g/L (SAC),0.3?g/L (E102),0.03?g/L (E124),0.1?g/L (E110) and 0.5?g/L (E123) and these values represent an advance in the current chromatographic analysis field. Thus the present method represents a big advance for measurement of the target analytes, especially for ACS-K, CYC and E133 in red wine.3) The method was successfully applied to the analysis and characterization of red wines from different countries of origin. The uncertainty of UPLC-MS/MS method was evaluated with metrology knowledge. The mathematical model of uncertainty was established and the different component of uncertainty was assessed in detail, finally expanded uncertainty was 6.0%(k=2) with mathematical calculation.4) An original and highly efficient method to simultaneously determine nine sweeteners, including acesulfame, saccharin, cyclamate, sucralose, aspartame, dulcin, alitame, neohesperidine dihydrochalcone and neotame, in spirits has been established using high performance liquid chromatography with diode array detector tandem charged aerosol detector(HPLC-DAD-CAD). The best separation condition was confirmed that nine analytes were separated within 25min using a BEH Cis column(2.1×100 mm,1.7?m) with a linear gradient elution program and the mobile phase A was methanol and the mobile phase B was 10 mmol/L ammonium acetate solution.5) The method has been evaluated on several validation parameters such as linearity, detection limit and recovery. Calibration curves were correlation coefficients (y2) better than 0.990 for all sweeteners within a studied range of concentrations (0.5-50mg/L). The recoveries at the tested concentrations for all sweeteners were in the range of 88.2%-99.9%, with relative standard deviations 0.4%-3.1%. The method is originally designed, simple, speedy, and successfully applied to the analysis and characterization of China spirits. The uncertainty was evaluated and contained six main source, including reference material, preparation of standard solution, standard curve, sample preparation, repeatability and recovery.