首页|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

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

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

freeze grindingheadspacegas chromatography-mass spectrometryfood packaging paperN-methylpyrrolidone

王颖、边照阳、王庆华、包毅、何屹、缪昊天、范子彦、唐纲岭

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国家烟草质量监督检验中心,郑州 450001

云南中烟工业有限责任公司,昆明 650231

四川三联新材料有限公司,成都 610000

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

2024

理化检验-化学分册
上海材料研究所

理化检验-化学分册

CSTPCD北大核心
影响因子:0.647
ISSN:1001-4020
年,卷(期):2024.60(12)