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3‐(2‐Bromoacetamido)‐ N ‐(9‐ethyl‐9 H )‐carbazol fluorescent probe and its application for the determination of thiophenols in rubber products by HPLC with fluorescence detection and atmospheric chemical ionization mass spectrometry identification
Author(s) -
You Jinmao,
Dou Kun,
Song Cuihua,
Li Guoliang,
Sun Zhiwei,
Zhang Shijuan,
Chen Guang,
Zhao Xianen,
Hu Na,
Zhou Wu
Publication year - 2017
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201601166
Subject(s) - chemistry , detection limit , thiophenol , reagent , derivatization , fluorescence , chromatography , acetonitrile , analyte , aqueous solution , high performance liquid chromatography , analytical chemistry (journal) , mass spectrometry , organic chemistry , physics , quantum mechanics
A rapid, sensitive, and selective precolumn derivatization method for the simultaneous determination of eight thiophenols using 3‐(2‐bromoacetamido)‐ N ‐(9‐ethyl‐9 H )‐carbazol as a labeling reagent by high‐performance liquid chromatography with fluorescence detection has been developed. The labeling reagent reacted with thiophenols at 50°C for 50 min in aqueous acetonitrile in the presence of borate buffer (0.10 mol/L, pH 11.2) to give high yields of thiophenol derivatives. The derivatives were identified by online postcolumn mass spectrometry. The collision‐induced dissociation spectra for thiophenol derivatives gave the corresponding specific fragment ions at m/z 251.3, 223.3, 210.9, 195.8, and 181.9. At the same time, derivatives exhibited intense fluorescence with an excitation maximum at λ ex = 276 nm and an emission maximum at λ em = 385 nm. Excellent linear responses were observed for all analytes over the range of 0.033–6.66 μmol/L with correlation coefficients of more than 0.9997. Detection limits were in the range of 0.94–5.77 μg/L with relative standard deviations of less than 4.54%. The feasibility of derivatization allowed the development of a rapid and highly sensitive method for the quantitative analysis of trace levels of thiophenols from some rubber products. The average recoveries ( n = 3) were in the range of 87.21–101.12%.