title: Ultrasonic-assisted precolumn derivatization-HPLC determination of acrylamide formed in Radix Asparagi during heating process.
abstract: An ultrasonic-assisted precolumn derivatization-HPLC method was established and validated for the determination of acrylamide formed in traditional Chinese herb Radix Asparagi during heating process. This method entails extraction with water, ultrasonic-assisted derivatization with 2-mercaptobenzoic acid. The final extracted acrylamide derivative was separated on C(18) column by using a mixture of acetonitrile and acetic acid (1 gL(-1) water solution) (20:80, v/v) as mobile phase. The flow rate was 0.7 mL min(-1) and the detection wavelength was set at 238 nm. Factors influencing the derivative reaction were evaluated and the optimum derivatization conditions were as follows: molar ratio of derivative reagent to acrylamide was 35:1, pH 8-12, ultrasonic-assisted reaction time was 100 min. The calibration curve of acrylamide showed good linearity in the range of 0.015-4.5 microg mL(-1) with correlation coefficient of 0.9999. The limit of detection was estimated to be 25 microg kg(-1) based on the signal-to-noise ratio of 3 recorded at 238 nm. Recovery of acrylamide from the sample was 106.6+/-6.6%. Relative standard deviation of five duplicate determinations for the same sample solution was 1.59%.
authors.affiliation: College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding, China. shizhihong@hbu.edu.cn
authors.forename: Zhihong
authors.initials: Z
authors.lastname: Shi
authors.forename: Hongyi
authors.initials: H
authors.lastname: Zhang
authors.forename: Xi
authors.initials: X
authors.lastname: Zhao
mesh_terms: D000178:Acrylamides / Q000032:analysis*; D027761:Asparagus Plant / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid; D006358:Hot Temperature; D006863:Hydrogen-Ion Concentration; D007202:Indicators and Reagents; D015203:Reproducibility of Results; D013056:Spectrophotometry, Ultraviolet; D014465:Ultrasonics
chemical_list: D000178:Acrylamides; D007202:Indicators and Reagents