双固相萃取柱净化-超高效液相色谱法测定热加工食品中的丙烯酰胺

目的 建立热加工食品中丙烯酰胺的双固相萃取柱净化-超高效液相色谱检测方法。方法 称取0.5~2.0g样品，先采用乙腈提取，再经正己烷脱脂，提取液真空离心浓缩。联用HLB和MCX小柱对提取液进行净化，水和甲醇洗脱，再真空浓缩，滤膜过滤后，用超高效液相色谱法分离测定，检测波长为197nm，外标法定量。结果 在0.5～10.0μg/ml的范围内，方法线性关系良好，r=0.998 7，方法检出限（LOD）为37.8μg/kg，方法定量限（LOQ）为124.7μg/kg，加标量为200μg/kg，500μg/kg和1000μg/kg时，回收率分别为87.5%，94.2%和92.0%，对有证标准物质进行分析，丙烯酰胺结果处于证书范围内，相对标准差为4.36%。结论 该方法线性范围宽、准确、可靠，适合热加工类食品中丙烯酰胺的测定。

Determination of acrylamide in hot processed foods by double solid phase extraction columns purification combined with ultra-high performance liquid chromatography

Objective To establish a method for determination of acrylamide in hot processed foods by ultra-high performance liquid chromatography after double solid phase extraction column purification. Methods Sample weighed 0.5-2.0g was extracted with acetonitrile, degreased with n-hexane, and then concentrated by vacuum centrifugation. HLB and MCX cartridges were used separately for purification, and acrylamide was eluted with water and methanol, then concentrated by vacuum centrifugation. After the eluent was filtered, the acrylamide in the sample solution was separated and determined by ultra-high performance liquid chromatography. The detection wavelength was 197 nm and the quantification was based on the external standard curve. Results The linear relationship of the method was good in the range of 0.5-10.0 μg/ml, with the correlative coefficient of 0.9987. The limit of detection (LOD) was 37.8μg/kg, and the limit of quantification (LOQ) was 124.7μg/kg. When the spiked levels were 200μg/kg, 500μg/kg and 1000μg/kg, the recovery rates of the method were 87.5%, 94.2% and 92.0%, respectively. When analyzing the certified reference materials, the result was within the scope of the certificate, with the relative standard deviation of 4.36%. Conclusion This method is of a wide linear range, accurate, reliable, and suitable for the determination of acrylamide in hot processed foods.