食品科学 ›› 2020, Vol. 41 ›› Issue (16): 266-271.doi: 10.7506/spkx1002-6630-20190716-219

• 安全检测 • 上一篇    

热转换元素分析-同位素比质谱法测定低氘包装饮用水中氘含量

韩莉,刘迪,余婷婷   

  1. (湖北省食品质量安全监督检验研究院,湖北 武汉 430074)
  • 发布日期:2020-08-19
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFC1602302);湖北省食品药品监督管理局科研项目(201801017)

Determination of Deuterium Content in Packaged Drinking Water Labeled Low Deuterium by Thermal Conversion/Elemental Analysis-Isotope Ratio Mass Spectrometry

HAN Li, LIU Di, YU Tingting   

  1. (Hubei Institute of Food Quality and Safety Supervision and Inspectionn, Wuhan 430074, China)
  • Published:2020-08-19

摘要: 建立热转换元素分析-同位素比质谱联用(thermal conversion/elemental analysis-isotope ratio mass spectrometry,TC/EA-IRMS)检测低氘水中氘含量分析方法,用于低氘包装饮用水中氘含量的监督检测。水样采用0.22 μm微孔滤膜过滤样品适量,移取2 mL水样装满进样瓶,进样量0.1 μL,反应炉温度1 380 ℃,柱温箱温度85 ℃,载气He流速100 mL/min,每个水样进行4~6 次分析。测试样品瓶不留顶空和剔除第1个数据点可以避免样品瓶顶空体积和记忆效应对δ2H测定值的影响,从而提高计算得到的氘含量值的精度。该方法适用于12.624~155.760 μg/g范围内水中氘含量的测定,测量值与理论值的相对标准偏差低于0.6%。对同一低氘水样连续8 次测定值除第1个点后氘含量标准偏差(standard deviation,SD)为0.08 μg/g,30 d内分3 次测定同一低氘水样氘含量SD为0.086 μg/g,重复性和再现性好。不同仪器方法测定的低氘水样SD低于1 μg/g。检测8 个市售低氘包装饮用水,测定值和标识值不相符的现象明显。TC/EA-IRMS测定低氘水中氘含量分析方法可以为标识为低氘水的包装饮用水中氘含量的监管检测提供技术支撑和理论依据。

关键词: 氘含量;低氘包装饮用水;热转换元素分析-同位素比质谱联用;监管检测

Abstract: A method for the determination of deuterium content in drinking water labeled low deuterium by thermal conversion/elemental analysis-isotope ratio mass spectrometry (TC/EA-IRMS) was established. The water sample was filtered through a 0.22 μm filter membrane, and 2 mL of the sample was transferred to a vial. The sample volume was 0.1 μL. The reactor temperature was 1 380 ℃, the column temperature was 85 ℃, and the carrier gas flow rate was 100 mL/min. Each sample was analyzed 4 to 6 times. The accuracy of the calculated deuterium content was improved by eliminating the first data point and the top space of the sample vial to avoid the influence of the void space and memory effect on the measurement of δ2H. This method was suitable for the determination of deuterium content in drinking water within the range of 12.624–155.760 μg/g, and the relative standard deviation (RSD) between the measured and theoretical values was less than 0.6%. The relative deviation (SD) of deuterium content in one deuterium-depleted water sample was 0.08 μg/g for 8 consecutive measurements, and 0.086 μg/g for 3 measurements within 30 days, indicating good repeatability and reproducibility. The RSD for the determination of water samples with low deuterium content by different instrumental methods was lower than 1 μg/g. The deuterium contents of 8 deuterium-depleted packaged drinking waters were tested. Generally, the measured and labeled values were not consistent with each other. Determination of deuterium content in deuterium-depleted water by TC/EA-IRMS can provide technical support and a theoretical basis for supervision and testing of deuterium content in packaged drinking water labeled low deuterium.

Key words: deuterium content; deuterium-depleted packaged drinking water; thermal conversion/elemental analsis-isotopic ratio mass spectrometry; testing and supervision

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