固相萃取-高效液相色谱法测定白砂糖中丙烯酰胺

Determination of Acrylamide in Sugar by Solid Phase Extraction High Performance Liquid Chromatography

建立了固相萃取-高效液相色谱法测定白砂糖中丙烯酰胺助剂残留的方法。采用Oasis HLB和Ac- cBond ODS-C_(18)固相萃取柱对样品进行净化,在Spherisorb NH_2柱上以乙腈-水(体积比为75:25)为流动相进行分离,流速0.8mL/min,柱温25℃,检测波长200nm,对白砂糖中丙烯酰胺助剂残留进行了测定。方法的线性范围为25～1000μg/L,线性相关系数为0.9992。方法的检出限为6μg/L,低、中、高3个浓度水平的加标回收率为90.2%～93.8%,相对标准偏差<5.5%。该法用于白砂糖中丙烯酰胺的测定,结果令人满意。

A solid phase extraction-high performance liquid chromatography method for the determination of acrylamide in sugar was developed. The samples were extracted with water, enriched and cleaned up with Oasis HLB and AccBond ODS-C18 solid phase extraction cartridge. The chromatographic separation was carried out on a NH2 column with 75% acetonitrile water solution as the mobile phase, the flow rate was 0.8 mL/min and the detection wavelength was set at 200nm. The calibration curve of acrylamide showed good linearity in the range of 25～1000 μg/L with correlation coefficient of 0. 999 . The detection limit of the method was 6 μg/L （S/N=3）. The average recoveries at three levels ranged from 90.2% to 93.8% （n=5）,and the relative standard derivation was lower than 5.5 %.