固相萃取-高效液相色谱法快速测定食品中米酵菌酸残留

Fast Determination of Bongkrekic Acid in Foods Using Solid Phase Extraction-High Performance Liquid Chromatography

目的:建立应用固相萃取-高效液相色谱测定食品中米酵菌酸残留的方法。方法:样品经甲醇-氨水超声提取,混合型强阴离子(MAX)固相萃取柱净化,C18色谱柱(4.6mm×250mm,5μm)分离,以甲醇-水(78∶22,V/V,水用冰乙酸调pH至2.5)为流动相、267nm为定量波长,二极管阵列检测器分析。结果:米酵菌酸在0.300~19.278μg·mL^-1内线性良好,相关系数为0.9997。方法检出限为0.005mg·kg^-1,平均加标回收率为82.25%~94.61%,相对标准偏差(RSD)不大于4.11%(n=6)。结论:该方法简便、灵敏、准确、检出限低,回收率、精密度均满足食品中米酵菌酸残留快速测定的要求。

Objective: A method for the determination of bongkrekic acid (BA) in foods was developed using solid phase extraction (SPE)-high performance liquid chromatography. Method: Samples were ultrasonically extracted with a mixture of methanol and ammonia, the extract was cleaned up by mixed-mode anion exchange(MAX) SPE, separated on a C18 column using a mobile phase consisting of methanol and water(78 ∶ 22,V/V, water was adjusted to pH 2.5 with glacial acetic acid), the quantitative wavelength was 267 nm with diode-array detector. Result: There was a good linearity between the peak area of analyte and its concentration in the range of 0.300 ~ 19.278 μg·mL^-1, the correlation coefficient was 0.999 7. The limit of detection (LOD) of the method was 0.005 mg·kg^-1. The mean recoveries of BA from spiked samples were 82.25%~ 94.61% with relative standard deviation (RSD) less than 4.11%(n=6). Conclusion: This method is efficient, sensitive and accurate with low LOD and high recovery, can be used for the fast determination of BA in various food samples.