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顶空气相色谱法测定肟类EN螯合剂中残留溶剂

朱金寿 肖炳坤 缪潇瑶 杨芳 黄荣清

军事医学2025,Vol.49Issue(5):370-373,4.
军事医学2025,Vol.49Issue(5):370-373,4.DOI:10.7644/j.issn.1674-9960.2025.05.007

顶空气相色谱法测定肟类EN螯合剂中残留溶剂

Determination of residual solvents in amidoxime EN chelating agents by headspace gas chromatography

朱金寿 1肖炳坤 2缪潇瑶 2杨芳 3黄荣清2

作者信息

  • 1. 青海大学药学系,西宁 810016||军事科学院军事医学研究院,北京 100850
  • 2. 军事科学院军事医学研究院,北京 100850
  • 3. 青海大学药学系,西宁 810016
  • 折叠

摘要

Abstract

Objective To establish an analytical method for the determination of methanol and ethanol solvent residues in amidoxime EN chelating agents by headspace gas chromatography.Methods The samples were analyzed in a GC-2030 gas chromatograph system using a Shimadzu HS-20 fully automated headspace injector and quantified by an internal standard method.The samples were separated and detected by the DB-WAX capillary column with a flame ionization detector(FID).The thermostatic furnace temperature was 70 ℃ and the equilibrium time of the sample bottle was 30 min.The sample flow path temperature was 150℃ and the carrier gas was high pure nitrogen.As temperature programming,the initial column temperature of 40 ℃ lasted 9 min and increased to 200 ℃ at 40 ℃/min for 2 min.Results The peak areas of the residual solvents in EN chelator showed good linearity(R2>0.999)in the mass concentration range investigated,the detection limits of solvent methanol and ethanol were 0.25 μg/mL and 0.30 μg/mL respectively,and the limits of quantification were 1.25 μg/mL and 1.50 μg/mL,respectively.The recovery of residual solvent addition ranged from 97.10%to 102.23%,and the RSD value was less than 5.00%.Conclusion This method is sensitive enough to be used for the determination of solvent residues in amidoxime EN chelating agents.

关键词

顶空气相色谱法/全自动顶空进样器/内标法/肟类EN螯合剂/甲醇/乙醇

Key words

headspace gas chromatography/automatic headspace sampler/internal standard method/amidoxime EN chelating agent/methanol/ethanol

分类

化学

引用本文复制引用

朱金寿,肖炳坤,缪潇瑶,杨芳,黄荣清..顶空气相色谱法测定肟类EN螯合剂中残留溶剂[J].军事医学,2025,49(5):370-373,4.

军事医学

1674-9960

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