title: Determination of trace acrylamide in starchy foodstuffs by HPLC using a novel mixed-mode functionalized calixarene sorbent for solid-phase extraction cleanup.
abstract: In this paper, a rapid and effective HPLC method, using tetraazacalix[2]arene[2]triazine-modified silica gel (NCSi) as solid-phase extraction (SPE) sorbent, was developed for the purification and determination of trace acrylamide in starchy foodstuffs. The main influence factors of SPE including amount of NCSi sorbent, sample flow rate, and volume and composition of washing solution were investigated and evaluated in the sample pretreatment step. The optimized purification effect was achieved at the sample flow rate of 3 mL/min with 100 mg of NCSi and 2 mL of washing solution (water, 100%). The HPLC separation was carried out on a C18 column (250×4.6 mm i.d., 5 μm) with a mobile phase of methanol/water (10:90, v/v). The linear range of the calibration curve was 4-4000 ng/mL with s correlation coefficient of >0.9999. The intraday and interday RSDs (n=5) of peak areas of acrylamide were 0.22 and 0.90% and the intraday and interday RSDs (n=5) of retention times were 0.50 and 1.63%, respectively. In addition, overall recoveries through the extraction and NCSi-SPE purification ranged from 73.13 to 98%. Compared with the commercial SPE sorbents, NCSi featured excellent selectivity to retain polar and nonpolar interferences in the sample matrices. The improved method was simple, rapid, accurate, and promising for the determination of trace acrylamide in starchy foods with a complex matrix.
authors.affiliation: College of Chemistry and Molecular Engineering, Zhengzhou University , Zhengzhou 450001, People's Republic of China.
authors.forename: Wenfen
authors.initials: W
authors.lastname: Zhang
authors.forename: Zhifen
authors.initials: Z
authors.lastname: Deng
authors.forename: Wenjie
authors.initials: W
authors.lastname: Zhao
authors.forename: Ling
authors.initials: L
authors.lastname: Guo
authors.forename: Wei
authors.initials: W
authors.lastname: Tang
authors.forename: Huifang
authors.initials: H
authors.lastname: Du
authors.forename: Lin
authors.initials: L
authors.lastname: Lin
authors.forename: Qiong
authors.initials: Q
authors.lastname: Jiang
authors.forename: Ajuan
authors.initials: A
authors.lastname: Yu
authors.forename: Lijun
authors.initials: L
authors.lastname: He
authors.forename: Shusheng
authors.initials: S
authors.lastname: Zhang
mesh_terms: D020106:Acrylamide / Q000032:analysis* / Q000302:isolation & purification; D053000:Analytic Sample Preparation Methods; D047250:Calixarenes / Q000737:chemistry; D002273:Carcinogens / Q000032:analysis* / Q000302:isolation & purification; D002681:China; D002851:Chromatography, High Pressure Liquid; D004040:Dietary Carbohydrates / Q000032:analysis; D057140:Fast Foods / Q000032:analysis* / Q000191:economics; D005506:Food Contamination; D005513:Food Inspection / Q000379:methods*; D007202:Indicators and Reagents / Q000737:chemistry; D015416:Maillard Reaction; D058428:Silica Gel / Q000737:chemistry; D052616:Solid Phase Extraction; D013213:Starch / Q000737:chemistry; D014227:Triazines / Q000737:chemistry
chemical_list: D002273:Carcinogens; D004040:Dietary Carbohydrates; D007202:Indicators and Reagents; D014227:Triazines; D047250:Calixarenes; D020106:Acrylamide; D058428:Silica Gel; D013213:Starch
keywords: HPLC; SPE purification; acrylamide; starchy foodstuffs; tetraazacalix[2]arene[2]triazine-modified silica gel