汪宣,朱翔,徐继俊,徐文君.顶空气相色谱质谱法测定烟用纸张中4种甲基环硅氧烷[J].包装工程,2025,(5):158-165.
WANG Xuan,ZHU Xiang,XU Jijun,XU Wenjun.Determination of 4 Kinds of Methylcyclosiloxane in Paper for Cigarette by Headspace Gas Chromatography-mass Spectrometry[J].Packaging Engineering,2025,(5):158-165. |
| 顶空气相色谱质谱法测定烟用纸张中4种甲基环硅氧烷 |
| Determination of 4 Kinds of Methylcyclosiloxane in Paper for Cigarette by Headspace Gas Chromatography-mass Spectrometry |
| 投稿时间：2024-07-26 |
| DOI：10.19554/j.cnki.1001-3563.2025.05.020 |
| 中文关键词: 烟用纸张 甲基环硅氧烷 顶空气相色谱质谱 三相平衡 |
| 英文关键词: cigarette paper methylcyclosiloxane headspace gas chromatography-mass spectrometry three-phase equilibrium |
| 基金项目:上海烟草集团有限责任公司科技项目(K2023-2-027P) |
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| 中文摘要: |
| 目的 研究烟用纸张中六甲基环三硅氧烷(D3)、八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)及十二甲基环六硅氧烷(D6)的顶空气相色谱质谱检测法。方法 样品经90 ℃顶空平衡30 min后，以正硅酸四(三甲基硅)酯为内标，通过选择性离子检测(Selected Ion Monitor，SIM)模式对商标纸、内衬纸及接装纸中4种甲基环硅氧烷进行检测，并以内标法定量。结果 检出限为0.000 2~0.002 9 mg/m2，回收率为87.0%~104.2%，精密度为0.3%~7.7%。在顶空三相平衡状态下，气相组成中甲基环硅氧烷含量与原始烟用纸张或标准溶液中该组分含量成正比关系。典型样品中甲基环硅氧烷整体含量水平为商标纸>内衬纸>接装纸，检出值均小于欧盟0.1%(质量分数)的参考限值。结论 本研究建立一种烟用纸张中甲基环硅氧烷的稳定、高灵敏度的检测方法，并解析三相平衡原理，为进一步完善烟用纸张质量安全评价手段提供技术支撑。 |
| 英文摘要: |
| The work aims to develop a headspace gas chromatography-mass spectrometry (HS-GC-MS) method for the determination of hexamethyldisiloxane (D3), octamethyltrisiloxane (D4), decamethyltetrasiloxane (D5), and dodecamethylpentasiloxane (D6) in cigarette paper. The samples were equilibrated at 90 °C for 30 min in the headspace. Tetramethylsilane tetraethoxysilicate was used as the internal standard. The four kinds of methylcyclosiloxane in the trademark paper, inner liner paper and tipping paper were detected by selected ion monitoring (SIM) mode and quantified by the internal standard method. The detection limit was 0.000 2-0.002 9 mg/m2, the recovery rate was 87.0%-104.2%, and the precision was 0.3%-7.7%. Under the three-phase equilibrium state of headspace, the content of methylcyclosiloxanes in the gas phase was proportional to the content of the component in the original cigarette paper or standard solution. The overall content level of methylcyclosiloxanes in typical samples was in the order of trademark paper>inner liner paper>tipping paper, and the detected values were all less than the reference limit of 0.1% (mass fraction) in the EU. A stable and highly sensitive detection method for methylcyclosiloxanes in cigarette paper is established in this study, and the principle of three-phase equilibrium is analyzed, providing technical support for further improving the quality and safety evaluation methods of cigarette paper. |
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