加压毛细管电色谱法分离检测薯片中丙烯酰胺的含量

建立加压毛细管电色谱法检测薯片中丙烯酰胺含量的方法。该方法采用EP-100-20/45-3-C18毛细管色谱柱(总长度45 cm,有效长度20 cm,直径100μm,ODS填料3μm)进行分离,并对流动相中有机相比例、磷酸盐缓冲溶液浓度、分离电压等实验条件进行考察和优化。结果表明:在流动相为乙腈-15 mmol/L NaH2PO4(pH 4.7)缓冲盐溶液(15∶85,V/V),流动相流速为0.04 mL/min,分离电压为-2 kV,紫外检测波长为202 nm的条件下,薯片中的丙烯酰胺得到了良好地分离。方法在2.0～32μg/mL范围内线性关系良好,相关系数为0.999 4。丙烯酰胺检出限(RSN=3)为0.30μg/mL,平均回收率为95.3%～108.1%,相对标准偏差低于1.48%。该方法已经用于薯片中丙烯酰胺含量测定,结果良好。

Separation and Determination of Acrylamide in Potato Chips by Pressurized Capillary Electrochromatography

An efficient pressurized capillary electrochromatography (pCEC) method was developed for the determination of acrylamide in potato chips. The separation was performed on a reversed-phase EP-100-20/45-3-C18 capillary column (total length 45 cm, effective length 20 cm, diameter 100 μm, ODS packing 3 μm). Moreover, the mobile phase composition, the concentration of phosphate buffer, separation voltage and other experimental conditions were investigated and optimized, respectively. The mobile phase was composed of a mixture of acetonitrile and 15 mmol/L NaH2PO4 (pH 4.7) (15:85, V/V) at a flow rate of 0.04 mL/min. Under the optimal conditions (separation voltage ?2 kV, and UV detection wavelength 202 nm), the analyte was well separated. The linear range was 2.0–32 μg/mL with a correlation coefficient of 0.999 4. The detection limit (LOD) of acrylamide was 0.30 μg/mL (RSN = 3). The average recoveries were 95.3%–108.1%, with a relative standard deviation (RSD) less than 1.48%. The method has been used for the determination of acrylamide in potato chips with good results.