全自动固相萃取-超高效液相色谱法快速测定食品中米酵菌酸含量

目的]建立混合型强阴离子(MAX)全自动固相萃取富集净化,超高效液相色谱法快速检测食品中米酵菌酸残留量的方法。方法]采用C18色谱柱(250 mm×4.6 mm,5μm),以甲醇和1%乙酸为流动相,检测波长为267 nm。结果]米酵菌酸在0.1~40.0 mg/L线性良好,相关系数大于0.999 9。考察样品的提取条件及不同固相萃取小柱的净化效果表明,选择80%乙腈溶液(含2%氨水)为提取溶剂,超声提取30 min,MAX小柱富集净化,效果最佳。方法检出限为2.5μg/kg,平均回收率为90.11%~96.54%,相对标准偏差为3.05%。结论]采用自动固相萃取仪,使得前处理简单快速、重复性好,方法学验证表明该方法精确灵敏、回收率高,适用于食品中米酵菌酸残留量的快速测定。

Fast Determination of Bongkrekic Acid in Food by Auto Solid Phase Extraction-ultra High Performance Liquid Chromatography

Objective]The research aimed to establish a mixed-mode anion exchange(MAX)auto solid phase extraction(SPE)purification and ultra-high performance liquid phase chromatography for the rapid determination of bongkrekic acid(BKA)in food.Method]Using a C18col-umn(250 mm×4.6 mm,5 μm),with methanol and 1% acetic acid as mobile phase,the detection wavelength was 267 nm.Result]BKA had a good linearity between the concentration range of 0.1-40.0 mg/L,the correlation coefficient was more than 0.999 9.The extraction conditions of the samples and the purification effects of different solid phase extraction cartridges showed that the optimum conditions were as follows:80%acetonitrile solution(containing 2% ammonia)as the extraction solvent and ultrasonic extraction for 30 min,MAX column enrichment purifica-tion,the best effect.The detection limit was 2.5 μg/kg.The average recovery was 90.11% -96.54%.The relative standard deviation was 3.05%.Conclusion]SPE makes the pretreatment simple, rapid and reproducible.The methodological verification shows that the method is ac-curate,sensitive and has high recovery rate.It is suitable for the rapid determination of the acid residues in BKA in food.