Determination of halogens in organic compounds by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS)
Determination of halogens in organic compounds by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS)
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DOI：
10.1039/b306570g
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发表时间：
2003-12-01
影响因子：
3.4
通讯作者：
Hall, G
中科院分区：
文献类型：
--
作者：
Bu, XD;Wang, TB;Hall, G
研究了双聚焦扇形场高分辨率电感耦合等离子体质谱法（HR-ICP-MS）测定固体有机化合物和原料药中卤素元素（氟、氯、溴和碘）的亚ppm至百分比水平的可行性。将样品溶解在适当的溶剂中，然后在去离子水或5%（v/v）氢氧化铵中稀释。通过应用中等或高分辨率，与传统的四极杆ICP-MS系统相比，背景计数可以降低多达五个数量级。比较和评估了所有四种元素在不同溶剂中的信号灵敏度和记忆效应。该方法用于测定一系列有机化合物和Merck原料药中F、Cl、Br和I的亚ppm至百分比水平。发现结果与这些化合物或原料药的已知或理论值非常一致。溶液中F的检测限估计为5 μ g ml（-1）（中等分辨率），Cl、Br和I的检测限分别为3（高分辨率）、0.08（高分辨率）和0.03（高分辨率）ng ml（-1）。
The feasibility of the determination of sub ppm to percentage levels of halogen elements (fluorine, chlorine, bromine, and iodine) in solid organic compounds and drug substances by double focusing sector field high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) was investigated. Samples were dissolved in appropriate solvents and then diluted in either deionized water or 5% (v/v) ammonium hydroxide. By applying medium or high resolution, the background counts can be lowered by up to five orders of magnitude compared to conventional quadrupole ICP-MS systems. The signal sensitivities and memory effects of all four elements in different solvents were compared and assessed. The methods were applied to the determination of sub ppm to percentage levels of F, Cl, Br and I in a series of organic compounds and Merck drug substances. The results were found to be in excel lent-to-reasonable agreement with the known or theoretical values of these compounds or drug substances. The limit of detection in solution for F was estimated to be 5 mug ml(-1) (medium resolution), and for Cl, Br and I was 3 (high resolution), 0.08 (high resolution) and 0.03 (high resolution) ng ml(-1), respectively.