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Determination of total phthalates in edible oils by high‐performance liquid chromatography coupled with photodiode array detection
Author(s) -
Xie Qilong,
Sun Dekui,
Han Yangying,
Jia Litao,
Hou Bo,
Liu Shuhui,
Li Debao
Publication year - 2016
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.201501169
Subject(s) - chromatography , phthalate , chemistry , phthalic acid , detection limit , repeatability , extraction (chemistry) , derivatization , high performance liquid chromatography , hydrolysate , hydrolysis , organic chemistry
The previously reported procedure for the determination of the total phthalate in fatty food involved the extraction of phthalates using chloroform/methanol followed by the removal of the solvents before alkaline hydrolysis requiring 20 h and derivatization of phthalic acid. In this study, a phase‐transfer catalyst (tetrabutylammonium chloride) was used in the liquid–liquid heterogeneous hydrolysis of phthalates in oil matrix shortening the reaction time to within 25 min. The resulting phthalic acid in the hydrolysate was extracted by a novel molecular complex based dispersive liquid–liquid microextraction method coupled with back‐extraction before high‐performance liquid chromatography coupled with photodiode array detection. Under the optimal experimental conditions, the linearity of the method was in the range of 0.5–12 nmol/g with the correlation coefficients ( r ) >0.997. The detection limit (S/N = 3) was 0.11 nmol/g. Intraday and interday repeatability values expressed as relative standard deviation were 3.9 and 7.1%, respectively. The recovery rates ranged from 82.4 to 99.0%. The developed method was successfully applied for the analysis of total phthalate in seven edible oils.