目的 建立同时测定竹木砧板表层中46种溶剂残留量的顶空-气相色谱-质谱方法,为砧板产品中溶剂残留量的质量安全监控提供技术支持。方法 刮取砧板表面样品,采用顶空进样,HP-INNOWAX毛细管色谱柱分离,电子轰击源(EI)下选择离子(SIM)模式检测,外标法定量。结果 在优化的条件下,46种溶剂均能较好分离,在0.2~20 μg内呈现良好线性,相关系数(r2)大于0.996,在3个不同加标水平下平均回收率为86%~109%,RSD为1.4%~8.4%,检出限为0.007~0.097 mg/kg。结论 本方法准确、可靠、灵敏度高,检出限和精密度满足分析要求,适用于竹木砧板表层中46种溶剂残留量的测定。
Abstract
The work aims to establish a headspace gas chromatography-mass spectrometry method for determining the residual amounts of 46 solvents in surface layer of bamboo and wood cutting boards, to provide technical support for the quality and safety monitoring of solvent residues in surface layer of bamboo and wood cutting board products. A certain amount of surface samples were scraped from the cutting board and the headspace method was adopted for sample injection. An HP-INNOWAX capillary chromatography column was used for separation and the selective ion monitoring (SIM) mode under an electron bombardment source (EI) was used for detection. Then, the external standard method was used for quantification. Under the optimized conditions, all 46 solvents were well separated. The 46 solvents showed good linearity in the range of 0.2-20 μg, with a correlation coefficient r2 greater than 0.996. The average recoveries at three spiked levels ranged from 86% to 109%, the relative standard deviation ranged from 1.4% to 8.4%, and the detection limits ranged from 0.007 mg/kg to 0.097 mg/kg. This method is accurate, reliable and highly sensitive, with the detection limit and precision conforming to the analytical requirements. It is suitable for the determination of residual amounts of 46 solvents in surface layer of bamboo and wood cutting boards.
关键词
溶剂残留 /
竹木砧板表层 /
顶空-气相色谱-质谱法
Key words
solvent residue /
surface layer of bamboo and wood cutting boards /
headspace gas chromatography-mass spectrometry
中图分类号:
O657.63
TB487
TB484.2
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基金
广州市市场监督管理局科技计划项目(2025KJ03); 广州市科技计划项目(2023B04J0407); 广州市院士专家工作站(2024-D012)