| 引用本文: | 廖惠云,王珂清,庄亚东,刘英杰,沈晓晨,曹毅,李朝建,朱龙杰.气相色谱-质谱联用内标法测定干性食品包装纸中的N-甲基吡咯烷酮[J].包装工程,2013,34(21):6-11. |
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| 摘要: |
| 建立了气相色谱-质谱联用内标法测定干性食品包装纸中N-甲基吡咯烷酮的分析方法。采用超声提取为前处理方式,使用乙醇为溶剂,目标物用GC-MS 进行了测定,内标法定量。探讨了不同萃取溶剂对目标物的提取效率,优选了合适的提取溶剂用量,比较了不同样品的提取方式及条件;甄选出合适的内标物,确定了较佳的特征离子及其丰度比,分析了色谱柱流量、进样量及分流比对目标物分离的影响,得到了合适的色谱分析条件。在优化的实验条件下,目标物N-甲基吡咯烷酮在0. 02745 ~2. 196 mg/ L 范围内具有良好的线性关系,相关系数(R2 )为0. 9999,平均回收率为98. 36 % ~ 108. 29 %,相对标准偏差为3. 71% ~ 6. 05 %,检出限为0. 058mg/ kg,定量下限为0. 194 mg/ kg。该方法简便、快速、灵敏、准确,适合于干性食品包装纸中N-甲基吡咯烷酮的测定。 |
| 关键词: 气相色谱-质谱 食品包装纸 N-甲基吡咯烷酮 |
| DOI： |
| 分类号:TS206. 4 |
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| Determination of N-Methyl Pyrrolidone in Dry Food Wrappings by Gas Chromatography-Mass Spectrometry Based on Internal Standard |
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LIAO Hui-yun, WANG Ke-qing, ZHUANG Ya-dong, LIU Ying-jie, SHEN Xiao-chen, CAO Yi, LI Chao-jian, ZHU Long-jie
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Jiangsu Tobacco Industry Co. , Ltd. , Nanjing 210019, China
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| Abstract: |
| A gas chromatography-mass spectrometry method (GC-MS) based on internal standard was developed for rapid determination of N-methyl pyrrolidone (NMP) in dry food wrappings. The NMP was extracted from the sample by ultrasonic extraction. The final product was determined by GC-MS based on internal standard. Extraction efficiency of different solvents on target object was discussed; suitable solvent dosage was determined; extraction modes and conditions for different samples were compared; suitable internal standard object was selected; the characteristic ions and its abundance were determined; the influence of column flow, injection volume, and split ratio on separation of target object was analyzed and suitable chromatography conditions were obtained. The result showed that under the optimal conditions, the calibration range of NMP was 0. 02745 ~2. 196 mg/ L with a correlation coefficient of 0. 9999; the average recoveries were in the range of 98. 36% ~108. 29%; with relative standard deviations of 3. 71% ~6. 05%, the detection limit and quantitation limit of NMP were 0. 058 mg/ kg and 0. 194 mg/ kg respectively. The method was simple,rapid, sensitive, accurate, and suitable for rapid determination of NMP in dry food wrappings. |
| Key words: GC-MS N-methyl pyrrolidone dry food wrappings |
