[Objective] The aim was to evaluate the uncertainty of determining aspartame in beverage by high performance liquid chromatography （ HPLC）. [Method] The content of aspartame in beverage was determined by HPLC, then ...[Objective] The aim was to evaluate the uncertainty of determining aspartame in beverage by high performance liquid chromatography （ HPLC）. [Method] The content of aspartame in beverage was determined by HPLC, then the source of uncertainty in the whole determination process was analyzed, and each component of uncertainty was evaluated and combined. [ Result] Through 6 repeated determinations by the method in GB/T 22254-2008 ＂Determination of Aspartame in Food＂, the average content of aspartame in beverage was （0.806 ±0.038） g/kg, and k =2. The main sources of uncertainty to affect the process were the sample weighting process, the preparation process of standard solution introduced by sample constant volume and the uncertainty introduced by fitting standard curve. ①The uncertainty of standard work-solution. The combined uncertainty of standard work-solution was 0.013 9, among them the uncertainty introduced by standard sample purity was 0.005 8, the standard uncertainty introduced by standard material weighting was 1.49 ×10^4, the relative uncertainty introduced by glass apparatus calibration in the preparation process of aspartame standard reserving solution was 0. 007 88, and the uncertainty introduced by glass apparatus calibration in the preparation process of standard work-solution was 0. 009 9. ②The uncertainty introduced by the preparation process of sample specimen. Among them the relative standard uncertainty introduced by sample weighting process was 0. 009, and the uncertainty introduced by sample constant volume was 0.000 78. ③The uncertainty introduced by the fitting process of standard curve. Among them the relative uncertainty of curve fitting was 0.002 46, the uncertainty introduced by the determined results of aspartame was 0.017 0, the total combined standard uncertainty was 0.023 9, and the expanded standard uncertainty was 0.019. [ Conclusion] The uncertainty components of standard solution, standard curve and repeatability are the main sources of uncertainty, while those 展开更多
A method for the determination of dichlofluanid residue by Capillary Collumns Gas Chromatography was established in this study.Samples were extracted with acetone and subjected to through liquid-liquid extraction with...A method for the determination of dichlofluanid residue by Capillary Collumns Gas Chromatography was established in this study.Samples were extracted with acetone and subjected to through liquid-liquid extraction with N-hexane,and then they were cleanup with column that filled with florisil,subsequently separated by Capillary Column Gas Chromatography,and the electron capture detector （ECD） was used for detection.The detection limit of this method was 0.005 mg/kg （S/N=3）,and this method was rapid,sensitive and accurate,and was applied in the determination of dichlofluanid residue in soybean.展开更多
基金Supported by the Key Project of Science and Technology of Anhui Province(08010302216)~~
文摘[Objective] The aim was to evaluate the uncertainty of determining aspartame in beverage by high performance liquid chromatography （ HPLC）. [Method] The content of aspartame in beverage was determined by HPLC, then the source of uncertainty in the whole determination process was analyzed, and each component of uncertainty was evaluated and combined. [ Result] Through 6 repeated determinations by the method in GB/T 22254-2008 ＂Determination of Aspartame in Food＂, the average content of aspartame in beverage was （0.806 ±0.038） g/kg, and k =2. The main sources of uncertainty to affect the process were the sample weighting process, the preparation process of standard solution introduced by sample constant volume and the uncertainty introduced by fitting standard curve. ①The uncertainty of standard work-solution. The combined uncertainty of standard work-solution was 0.013 9, among them the uncertainty introduced by standard sample purity was 0.005 8, the standard uncertainty introduced by standard material weighting was 1.49 ×10^4, the relative uncertainty introduced by glass apparatus calibration in the preparation process of aspartame standard reserving solution was 0. 007 88, and the uncertainty introduced by glass apparatus calibration in the preparation process of standard work-solution was 0. 009 9. ②The uncertainty introduced by the preparation process of sample specimen. Among them the relative standard uncertainty introduced by sample weighting process was 0. 009, and the uncertainty introduced by sample constant volume was 0.000 78. ③The uncertainty introduced by the fitting process of standard curve. Among them the relative uncertainty of curve fitting was 0.002 46, the uncertainty introduced by the determined results of aspartame was 0.017 0, the total combined standard uncertainty was 0.023 9, and the expanded standard uncertainty was 0.019. [ Conclusion] The uncertainty components of standard solution, standard curve and repeatability are the main sources of uncertainty, while those
文摘A method for the determination of dichlofluanid residue by Capillary Collumns Gas Chromatography was established in this study.Samples were extracted with acetone and subjected to through liquid-liquid extraction with N-hexane,and then they were cleanup with column that filled with florisil,subsequently separated by Capillary Column Gas Chromatography,and the electron capture detector （ECD） was used for detection.The detection limit of this method was 0.005 mg/kg （S/N=3）,and this method was rapid,sensitive and accurate,and was applied in the determination of dichlofluanid residue in soybean.
