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                       Determination of N-Methylpyrrolidone in Food Packaging Paper by
                               Gas Chromatography-Mass Spectrometry with Freeze

                                                Grinding and Headspace


                        WANG Ying , BIAN Zhaoyang , WANG Qinghua , BAO Yi , HE Yi , MIAO Haotian ,
                                                                             3*
                                                                    2
                                                                                    3
                                                    1
                                   1
                                                                                                   3
                                                 FAN Ziyan , TANG Gangling 1
                                                           1
               (1. China National Tobacco Quality Supervision and Test Center, Zhengzhou 450001, China; 2. China Tobacco Yunnan Co., Ltd.,
                           Kunming 650231, China; 3. Sichuan San Lian New Materials Co., Ltd., Chengdu 610000, China)
                  Abstract: A method for determination of N-methylpyrrolidone (NMP) in food packaging paper by gas chromatography-
              mass spectrometry with freeze grinding and headspace was proposed. The food packaging paper sample was frozen and ground,
              and 1 g of ground sample was taken and placed in a 20 mL-headspace vial. 1 mL of glycerol triacetate was added, and 100 µL of
              1 g· L −1  NMP-d 9  internal standard solution was added. The mixture was separated on a HP-INNOWAX chromatographic column
              according to the column heating program. Selected ion monitoring (SIM) mode was adopted in mass spectrometry analysis, and the
              matrix matching method was used for quantitative analysis. As shown by the results, linear relationship between the ratios of the
                                                                                                            −1
              corresponding peak area to the internal standard peak area and mass fractions of NMP was kept in the range of 5-500 mg · kg  ,
              with detection limit (3S/N) of 1. 07 mg · kg  −1 .  Test for recovery was made by the standard addition method, giving results in
              the range of 98. 8%-100%, with RSDs (n=6) of the determined values less than 2. 0%. This method was used for the analysis
              of 36 samples of food packaging paper, and NMP in 15 samples was detected, with detection amounts in the range of 26. 3-
                         −1
              351. 0 mg · kg  .
                  Keywords: freeze grinding; headspace; gas chromatography-mass spectrometry; food packaging paper; N-methylpyrrolidone

































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