胡伟,马俊辉,张晓飞,徐文,周良春,李双琦.ASE-GC-NCI-MS测定食品接触塑料及纸制品中的短链氯化石蜡[J].包装工程,2019,40(13):67-75.
HU Wei,MA Jun-hui,ZHANG Xiao-fei,XU Wen,ZHOU Liang-chun,LI Shuang-qi.Determination of Short Chain Chlorinated Paraffins in Food Contact Plastic and Paper Products by ASE-GC-NCI-MS[J].Packaging Engineering,2019,40(13):67-75. |
| ASE-GC-NCI-MS测定食品接触塑料及纸制品中的短链氯化石蜡 |
| Determination of Short Chain Chlorinated Paraffins in Food Contact Plastic and Paper Products by ASE-GC-NCI-MS |
| 投稿时间：2019-03-18 修订日期：2019-07-10 |
| DOI：10.19554/j.cnki.1001-3563.2019.13.010 |
| 中文关键词: 短链氯化石蜡 气相色谱-负化学电离源质谱法 快速溶剂萃取 总体响应因子 食品接触塑料 纸制品 |
| 英文关键词: short chain chlorinated paraffins gas chromatography-negative chemical ionization-mass spectrometry accelerated solvent extraction total response factor food contact plastic paper products |
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| 目的 建立用于食品接触塑料及纸制品中短链氯化石蜡（SCCPs）含量测定的快速溶剂萃取-气相色谱-负化学电离源质谱法（ASE-GC-NCI-MS）。方法 采用加速溶剂萃取法对食品接触塑料及纸制品中的SCCPs进行处理，萃取溶剂为正己烷-二氯甲烷，萃取温度为80 ℃，静态萃取时间10 min；采用浓硫酸净化法对萃取溶液进行净化处理；采用气相色谱-质谱法在负化学电离模式、全扫描模式、离子源温度为180 ℃等条件下对样品中的SCCPs进行定性与定量测定。结果 氯的质量分数在58.7%~64.3%范围内时，SCCPs的总体响应因子与实测氯含量呈良好的线性关系，线性相关系数R2为0.9765，检出限为20 mg/kg，加标回收率为86.3%~95.3%，相对标准偏差（RSD）为3.3%~5.2%（日内），4.8%~8.1%（日间）。结论 该方法操作简便、准确度好、灵敏度高、检出限低，可用于食品接触塑料及纸制品中SCCPs的实际检测。 |
| 英文摘要: |
| The work aims to establish the accelerated solvent extraction-gas chromatography-negative chemical ioni-zation-mass spectrometry (ASE-GC-NCI-MS) used to determine short chain chlorinated paraffins (SCCPs) in food contact plastic and paper products. Accelerated solvent extraction was used to extract SCCPs from food contact plastic and paper products. The extraction solvent was n-hexane-dichloromethane, the extraction temperature was 80 ℃, and the static extraction time was 10 min. Then, concentrated sulfuric acid was adopted to purify the extracted solution. SCCPs in the sample were qualitatively and quantitatively detected by gas chromatography-mass spectrometry under negative chemical ionization mode, full scan mode, and at 180 ℃ (ionization source temperature). In the range of 58.7%~64.3% (mass fraction) chlorine, the total response factor of SCCPs and measured chlorine content had a good linear relationship, with a linear correlation coefficient (R2) of 0.9765. The limit of detection was 20 mg/kg. The recoveries ranged from 86.3% to 95.3%, with relative standard deviations (RSD) of 3.3%~5.2% (intra-day) and 4.8%~8.1% (inter-day). Featured by convenient operation, good accuracy, high sensitivity and low detection limit, the proposed method can be used for the detection of SCCPs in food contact plastic and paper products. |
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