同位素 ›› 2020, Vol. 33 ›› Issue (5): 304-311.DOI: 10.7538/tws.2020.33.05.0304

• 稳定同位素技术在食品安全检测中的应用专辑 • 上一篇    下一篇

敌百虫-D6同位素丰度的快速测定及计算

盛立彦;李美华;杜晓宁   

  1. 上海化工研究院有限公司 上海稳定同位素工程技术研究中心,上海200062
  • 出版日期:2020-10-20 发布日期:2020-10-28

Rapid Determination and Calculation of Isotope Enrichment of Trichlorfon-D6

SHENG Liyan;LI Meihua;DU Xiaoning   

  1. Shanghai Research Institute of Chemical Industry Co. Ltd., Shanghai Engineering Research Center of Stable Isotope, Shanghai 200062, China
  • Online:2020-10-20 Published:2020-10-28

摘要:

在敌百虫-D6行业标准规定的同位素丰度测试方法中,采用蠕动泵引入样品耗时长且操作较依赖主观判断,结果计算的“质量簇”方法则较为繁琐。为了在保证测试效果的前提下提高样品测试效率,本文采用液相色谱代替标准方法中的蠕动泵引入样品,并用ESI离子源质谱测定敌百虫-D6的同位素丰度,以线性公式代替“质量簇”法进行同位素丰度的快速计算并与标准方法进行对照验证。在样品浓度0.1 g/L及以上时,测定结果与标准方法偏差≤0.2 atom%D,重现性RSD≤0.1%。结果表明,该方法准确、精密,能够快速地对敌百虫-D6同位素丰度进行测定及计算。

关键词: 敌百虫-D6, 同位素丰度, 液质联用, 质量簇

Abstract:

As the trade standard of Trichlorfon-D6 requires, when determining isotope enrichment of trichlorfon-D6, sample solution is introduced to ESI-MS by syringe pump, and data are processed by the “Mass Cluster” method to calculate the result. In this study, in order to overcome the time-consuming shortcoming in both sample introduction and data processing progress, liquid chromatography was used instead of syringe pump to introduce sample while a simplified formula was deducted to replace the “mass clusters” during data processing. Then this rapid method is verified, compared to the standard method. When the concentration of sample solution was above 0.1 g/L, isotope enrichment was within ±0.2 atom%D of the corresponding results acquired by the standard method with RSD less than 0.1%. The results showed that this new method was accurate and precise, fully competent of rapid determination and calculation of isotope enrichment of trichlorfon-D6.

Key words: Trichlorfon-D6, isotope enrichment, LC-MS, mass cluster