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• 安全检测 •    下一篇

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方法研究

韩莉,刘迪,余婷婷   

  1. 湖北省食品质量安全监督检验研究院
  • 收稿日期:2019-07-17 修回日期:2020-05-25 出版日期:2020-08-25 发布日期:2020-08-19
  • 通讯作者: 韩莉 E-mail:447605531@qq.com
  • 基金资助:
    食品中重点危害物质高效识别和确证关键技术研究-危害物高分辨质谱全谱识别技术与多级质谱数据库构建;稳定同位素溯源技术识别食品中甲醛来源

Study on determination of deuterium content in packaged drinking water with low deuterium label by TC/EA-IRMS

HAN Li,Di Liu,   

  • Received:2019-07-17 Revised:2020-05-25 Online:2020-08-25 Published:2020-08-19
  • Contact: HAN Li E-mail:447605531@qq.com

摘要: 建立了热转换元素分析-同位素比质谱联用(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,反应炉温度为1380 ℃,柱温箱温度85 ℃,载气氦气流速100 mLmin-1,每个水样进行4~6次分析。测试样品瓶不留顶空和剔除第一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。该方法适用于氘含量12.624~155.760 ppm范围内低氘水中氘含量的测定,测量值与理论值的相对标准偏差RSD低于0.6%。对同一低氘水样连续8次测定的值除第一个点后氘含量标准偏差SD为0.08 ppm,30天内分3次测定同一低氘水样氘含量标准偏差SD为0.086 ppm,重复性和再现性好。不同仪器方法测定的低氘水样相对标准偏差SD低于1 ppm。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同位素质谱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 with low deuterium label by TC/EA-IRMS was established. The water sample was filtered by 0.22 micron filter membrane, and 2mL water sample was removed and filled with sample bottle. The sample quantity was 0.1μL. The reactor temperature was 1380℃, the column temperature was 85℃, and the carrier gas flow rate was 100mLmin-1. Water sample was analyzed 4 to 6 times.The accuracy of the deuterium content can be improved by eliminating the first data point and eliminating the top space of the sample bottle. This method is suitable for the determination of deuterium content in deuterium-depleted water within the range of deuterium content 12.624~155.760 ppm, and the RSD of measured value and theoretical value is less than 0.6%. The SD of deuterium content in the same deuterium-depleted water sample was 0.08 ppm for 8 consecutive measurements. The SD of deuterium content in the same deuterium-depleted water sample was 0.086 PPM for 3 measurements within 30 days.This method for the determination of deuterium content in deuterium-depleted water has good repeatability and reproducibility. The relative standard deviation SD of water samples with low deuterium determined by different instrument methods is less than 1ppm. The deuterium content of 8 deuterium-depleted packaged drinking water was tested.It was general that the measured value and labelled value were not consistent with each other. Determination of deuterium content in deuterium-depleted water by TC/EA-IRMS isotope mass spectrometry can provide technical support and theoretical basis for supervision and testing of deuterium content in packaged drinking water labeled with low deuterium.

Key words: deuterium content, deuterium-depleted packaged drinking water, Thermal conversion/elemental analsis-isotopic ratio mass spectrometry(TC/EA-IRMS), testing and supervision

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