硅烷化衍生和气相色谱/质谱法分析测定水样中的痕量氟。
Determination of trace fluoride in water samples by silylation and gas chromatography/mass spectrometry analysis.
机构信息
Key Laboratory of Organosilicon Chemistry and Material Technology, Hangzhou Normal University, Hangzhou, 311121, PR China.
出版信息
Rapid Commun Mass Spectrom. 2021 Jun 15;35(11):e9089. doi: 10.1002/rcm.9089.
RATIONALE
Due to the ubiquity of fluorides and the small gap between a safe dose and a harmful one, it is necessary to develop a robust analytical method for determination of fluoride ions in various water samples with complex matrices.
METHODS
Silylation of the fluoride ion was carried out by treatment with hydrochloric acid and phenyldimethylchlorosilane at room temperature. The formed phenyldimethylfluorosilane was detected by gas chromatography/mass spectrometry (GC/MS).
RESULTS
Under the optimized conditions, linearity in the analytical method ranged from 0.050 to 5.0 μg/mL for the fluoride ion with R >0.9999. Reasonable reproducibility was obtained with the intraday relative standard deviation (RSD) (N = 5) of 2.04% and interday RSD (N = 5) of 3.75% at the concentration of 0.10 μg/mL. The developed method has been successfully applied to determine the fluoride ion in real water samples, including waste water samples, with the recovery between 81.12% and 113.04%.
CONCLUSIONS
A robust method for the determination of the fluoride ion has been developed by silylation with phenyldimethylchlorosilane and GC/MS analysis. The established method showed good anti-interference and precision, and it has been applied for determination of the fluoride ion in various water samples.
原理
由于氟化物的普遍存在以及安全剂量和有害剂量之间的微小差距，因此有必要开发一种强大的分析方法，以测定各种复杂基质水样中的氟离子。
方法
室温下用盐酸和二甲基苯基氯硅烷处理氟离子进行硅烷化。通过气相色谱/质谱（GC/MS）检测形成的二甲基苯基氟硅烷。
结果
在优化条件下，氟离子的分析方法在 0.050 至 5.0 μg/mL 范围内呈线性，相关系数（R）>0.9999。在 0.10 μg/mL 浓度下，日内相对标准偏差（RSD）（N=5）为 2.04%，日间 RSD（N=5）为 3.75%，得到了合理的重现性。该方法已成功应用于测定实际水样中的氟离子，包括废水样，回收率在 81.12%至 113.04%之间。
结论
通过二甲基苯基氯硅烷硅烷化和 GC/MS 分析，建立了一种测定氟离子的可靠方法。所建立的方法具有良好的抗干扰性和精密度，已应用于各种水样中氟离子的测定。
Zotero 插件