用GC-MS测定紫外线滤光片和激素的分析方法开发过程中硅烷化作用的评价

IF 1.1 Q4 CHEMISTRY, ANALYTICAL Brazilian Journal of Analytical Chemistry Pub Date : 2023-08-29 DOI:10.30744/brjac.2179-3425.ar-32-2023
Jean Paulo Coll, Michele da Cunha, Maria Alice Amaral, Maurício Padilha, G. da Silva, Daniel Arsand, P. S. Sanches Filho
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引用次数: 0

摘要

本研究的目的是优化衍生化(硅基化)与MSTFA (n -甲基- n -(三甲基硅基)三氟乙酰胺)相结合的色谱分析方法,并采用气相色谱-质谱联用(GC-MS)对激素和紫外滤光剂进行选择性测定,评价衍生化对色谱响应的影响。所开发的定性分析方法(扫描模式)可以更准确地识别分析物,光谱相似度优于80%。检测限为0.1 ~ 1.3µg L-1,定量限为0.3 ~ 4.2µg L-1。该定量方法采用硅基化与色谱法在SIM模式下进行测定,结果表明该方法精确(相对标准偏差<7.2%)、准确(相对误差<2.0%),模型不缺乏拟合,相关系数线性值大于0.9,符合监管机构的要求和标准。
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Evaluation of the Effect of Silylation in the Development of an Analytical Method for the Determination of UV Filters and Hormones by GC-MS
The objective of this work was to optimize a chromatographic method, combining derivatization (silylation) with MSTFA (N-methyl-N-(trimethylsilyl)trifluoracetamide) and analysis by gas chromatography coupled to mass spectrometry (GC-MS), for the determination of hormones and UV filters selectively, evaluating the effect of derivatization on the chromatographic response. The method developed for the qualitative analysis (SCAN mode) allowed the identification of the analytes more accurately, with similarities of the spectra superior to 80%. The limits of detection and quantification ranged from 0.1 to 1.3 µg L-1 and 0.3 to 4.2 µg L-1 respectively. The quantitative method, combined silylation with chromatographic determination in SIM mode, proved to be precise (Relative standard deviation <7.2%) and exact (relative error <2.0%), with models without lack of fit, and with correlation coefficients linear values greater than 0.9, in accordance with the requirements and standards of the regulatory bodies.
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来源期刊
CiteScore
1.60
自引率
14.30%
发文量
46
期刊介绍: BrJAC is dedicated to the diffusion of significant and original knowledge in all branches of Analytical Chemistry, and is addressed to professionals involved in science, technology and innovation projects at universities, research centers and in industry.
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