| 梁美宜， 莫锡乾， 曾绮莹， 黄静娴.顶空-气相色谱法快速测定油脂中的4种卤代甲烷[J].中国油脂,2026,51(7):.[LIANG Meiyi, MO Xiqian, ZENG Qiying, HUANG Jingxian.Rapid determination of four halomethanes in oils by headspace-gas chromatography[J].China Oils and Fats,2026,51(7):.] |
| 顶空-气相色谱法快速测定油脂中的4种卤代甲烷 |
| Rapid determination of four halomethanes in oils by headspace-gas chromatography |
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投稿时间：2025-10-15 修订日期：2026-02-27 录用日期：2026-01-07
出版日期：2026-07-20
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| DOI：10.19902/j.cnki.zgyz.1003-7969.250456 |
| 中文关键词: 顶空-气相色谱法 油脂 卤代甲烷 快速测定 |
| 英文关键词:headspace-gas chromatography oil halomethane rapid determination |
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| 中文摘要: |
| 旨在为油脂中卤代甲烷的测定提供技术支撑，建立了顶空-气相色谱法对油脂中的4种卤代甲烷（三氯甲烷、四氯化碳、二氯一溴甲烷和一氯二溴甲烷）进行快速测定的方法。2.5 g样品在95 ℃下加热平衡30 min，自动顶空进样（进样时间4 s，进样量250 μL），目标物经CD-5石英毛细管色谱柱(30 m×0.32 mm，0.25 μm)分离，使用电子捕获检测器进行测定。4种卤代甲烷的空白基质曲线在2~200 μg/kg范围内呈良好线性关系，决定系数在0.998 3~0.999 9之间，方法检出限和定量限分别为0.6~2.0 μg/kg和2.0~5.0 μg/kg；在1、2、10倍定量限的加标水平下，6次平行测定结果的平均回收率为89.9%~110.0%，相对标准偏差为3.17%~6.59%。综上，该方法简单高效，准确度高、重复性好、灵敏度高，可用于油脂中4种卤代甲烷的快速测定。 |
| 英文摘要: |
| To provide technical support for the determination of halomethanes in oils, a headspace-gas chromatography method was established for the rapid determination of four halomethanes (trichloromethane, carbon tetrachloride, bromomonochloromethane and dibromochloromethane) in oils. The samples (2.5 g) were heated at 95 ℃ for 30 min and then automatically filled with headspace (injection time 4 s, injection volume 250 μL). The analytes were separated by CD-5 quartz capillary column (30 m×0.32 mm, 0.25 μm) and quantified by electron capture detector. The blank matrix curves of the four halomethanes showed a good linear relationship in the range of 2-200 μg/kg, while the correlation coefficients ranged from 0.998 3-0.999 9. The limit of detection (LOD) and limit of quantification (LOQ) for the method were 0.6-2.0 μg/kg and 2.0-5.0 μg/kg, respectively.The average recoveries of six parallel determination results were ranged from 89.9% to 110.0% with the relative standard deviations were 3.17%-6.59% at the spiked levels of 1, 2, 10 times of LOQ. To sum up, the method is simple, efficient, and exhibits high accuracy, good reproducibility and high sensitivity, making it suitable for rapid determination of four halomethanes in oils. |
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