高效液相色谱-电感耦合等离子体质谱联用测定食品中的二氧化硫含量
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湖北省食品质量安全监督检验研究院

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国家重点基础研究发展计划(973计划)


Determination of Sulfur Dioxide Content in Food by High Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry
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    摘要:

    为解决复杂基质食品中二氧化硫含量测定基质干扰大,难以精准测定的问题,建立基于高效液相色谱-电感耦合等离子体质谱串联(High Performance Liquid Chromatography - Inductively Coupled Plasma Mass Spectrometry, HPLC-ICP-MS/MS)的二氧化硫测定新方法。通过实验确定最佳二氧化硫检测目标物、碰撞池气体流量等实验参数,同时对甲醛吸收液质量浓度、进样体积、流动相pH值及其浓度、流动相流速等实验条件进行优化。结果表明,在0.0~20.0 mg·L-1范围内,待测物响应信号与二氧化硫浓度呈现良好线性关系(R2=0.9999),背景等效浓度(BEC)为7.4 μg·L-1,检出限为3 mg·kg-1,定量限为9 mg·kg-1。该法可实现对葡萄酒、酱腌菜和果脯类中的二氧化硫残留量的准确测定,以酵母抽提物为基质的不同浓度样品加标回收率在93.0%~105.9%之间,相对标准偏差(RSD)均低于5%。该方法有效克服复杂基质干扰、缩短检验时长,着重增强方法的适用性、准确性以及灵敏度,实现食品中二氧化硫残留的精准测定,为日常监管提供高效、便捷的技术支持,助力构建更完善的食品安全保障体系。

    Abstract:

    High performance liquid Chromatography-Inductively Coupled plasma mass spectrometry tandem(HPLC-ICP-MS/MS) method was established to determine the content of sulfur dioxide in food. Experimental parameters such as the target substance for sulfur dioxide detection and the gas flow rate in the collision cell were determined through testing. At the same time, the experimental conditions of formaldehyde absorption liquid mass concentration, injection volume, mobile phase pH value and concentration, and mobile phase flow rate were optimized. The results showed that there was a good linear relationship between the response signal of the analyte and the concentration of sulfur dioxide within the range of 0.0~20.0 mg·L-1 (R2=0.9999). The background equivalent concentration (BEC) was 7.4 μg·L-1, the detection limit was 3 mg·kg-1, and the quantification limit was 9 mg·kg-1. This method can accurately determine the residual sulfur dioxide in wine, pickled vegetables, and dried fruits. The recovery rates of different concentration samples based on yeast extract ranged from 93.0% to 105.9%, with relative standard deviations (RSD) below 5%. This method effectively overcomes complex matrix interference, shortens inspection time, and focuses on enhancing the applicability, accuracy, and sensitivity of the method, achieving precise determination of sulfur dioxide residues in food, providing efficient and convenient technical support for daily supervision, and helping to build a more complete food safety guarantee system.

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  • 收稿日期:2025-05-09
  • 最后修改日期:2025-06-24
  • 录用日期:2025-06-30
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