The Research On Illegal Additives And Characteristic Compounds In Chinese Spirits By Various Mass Spectrum Detection Technologies

Chinese spirits are the necessary drinks in dinner table. In recent years, Chinese spirits facing serious quality problems, such as phthalate esters contamination, illegal artificial sweeteners, and other quality problems. So, phthalate esters, artificial sweeteners and flavor compounds have become the main monitoring targets for liquid quality control. In view of the above problems, we studied the three kinds of substances by various mass spectrum detection technologies. The main content of my work is as follow:1. An isotope dilution mass spectrometry technique has been developed for the high accuracy analysis of 16 phthalate esters in Chinese spirits. From the sample treatment point of view, the traditional liquid-liquid extraction was improved, Chinese spirits need to remove the ethanol by a stream of nitrogen with boiling water bath, and then extract twice with n-hexane. The operation is simple, fast and low organic solvent consumption. In terms of detection, the multiple reaction monitoring mode was used. This acquistion mode has the advantages of high sensitivity and strong specificity. The method detection limits ranged 0.1 ng g-1 to 10.0 ng g-1. From the quantitative point of view, an isotope dilution mass spectrometry method has been developed by using 16 corresponding deuterated phthalate esters as internal standards, and matrix-matched calibration standards were also used in the quantitative analysis. The precision and accuracy of the method were effectively validated by standard addition recovery test, the recoveries of 16 analytes ranged from 94.3% to 105.3% with RSD<6.5%. This method can meet the limited detection of PAEs in Chinese spirits.2. A rapid screening method was developed for determination and confirmation of seven artificial sweeteners in Chinese spirits by applying direct analysis in real time ion source-tandem mass spectrometry. The spirits can be detected directly by mass spectrometry, which greatly save the time for sample preparation. In terms of detection, the multiple reaction monitoring mode was high sensitivity with the method detection limits of 0.8 μg L-1-80 μg L-1. The advantage of specificity can effectivity rule out false positive results. From the quantitative point of view, the matrix calibration work solution can effectively improve the accuracy of the quantitative results by eliminating the matrix interference.3. We analyze flavor compounds of Chinese spirits combining the high resolution gas chromatography quadrupole time-of-flight tandem mass spectrometry and the automated direct immersion solid-phase microextraction technology. We found 104 common flavor compounds between four Chinese mild flavour spirits and 13 significant difference between two brands after chemometric analysis using high efficient Mass Profiler Professional software. The method is automatic, simple, high efficient and accuracy, which can meet the requirement of the analysis of trace flavor compounds in spirits, and provide a reference value for Chinese spirits in identification.These methods will have important significance for monitoring and improving the quality of liquor, and protecting the consumers’ rights and interests.