冷冻研磨-顶空-气相色谱-质谱法测定食品包装纸中N-甲基吡咯烷酮的含量  

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

作　　者：王颖[1] 边照阳[1] 王庆华 包毅 何屹 缪昊天 范子彦[1] 唐纲岭[1] WANG Ying;BIAN Zhaoyang;WANG Qinghua;BAO Yi;HE Yi;MIAO Haotian;FAN Ziyan;TANG Gangling(China National Tobacco Quality Supervision and Test Center,Zhengzhou 450001,China;China Tobacco Yunnan Co.,Ltd.,Kunming 650231,China;Sichuan San Lian New Materials Co.,Ltd.,Chengdu 610000,China)

机构地区：[1]国家烟草质量监督检验中心,郑州450001 [2]云南中烟工业有限责任公司,昆明650231 [3]四川三联新材料有限公司,成都610000

出　　处：《理化检验（化学分册）》2024年第12期1288-1292,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：提出了冷冻研磨-顶空-气相色谱-质谱法测定食品包装纸中N-甲基吡咯烷酮(NMP)含量的方法。将食品包装纸样品进行冷冻研磨,取1 g研磨后的样品置于20 mL顶空瓶中,加入1 mL三乙酸甘油酯,再加入1 g·L^(-1)NMP-d9内标溶液100μL,在HP-INNOWAX色谱柱上按照柱升温程序分离,质谱分析采用选择离子监测(SIM)模式,基质匹配法定量。结果表明,NMP的质量分数在5~500 mg·kg^(-1)内和NMP与内标峰面积之比呈线性关系,检出限(3S/N)为1.07 mg·kg^(-1)。按照标准加入法进行回收试验,回收率为98.8%~100%,测定值的相对标准偏差(n=6)均小于2.0%。方法用于36个食品包装纸样品的分析,其中15个样品中检出NMP,检出量为26.3~351.0 mg·kg^(-1)。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 100µL of 1 g·L^(-1) NMP-d9 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 corresponding peak area to the internal standard peak area and mass fractions of NMP was kept in the range of 5-500 mg·kg^(-1),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 26.3-351.0 mg·kg^(-1).

关 键 词：冷冻研磨 顶空 气相色谱-质谱法 食品包装纸 N-甲基吡咯烷酮 

分 类 号：O657.63[理学—分析化学]