超高效液相色谱-串联质谱法测定广西生榨米粉中的米酵菌酸

Determination of Bongkrekic Acid in Guangxi Fresh Rice Noodles by Ultra Performance Liquid Chromatograghy-Tandem Mass Spectrometry

目的:建立混合型阴离子固相萃取富集净化,超高效液相色谱-串联质谱测定广西生榨米粉中米酵菌酸的方法,并初步评估生榨米粉被米酵菌酸污染的风险。方法:以广西生榨米粉作为研究对象,用混合型阴离子交换小柱净化,梯度洗脱(0.1%甲酸水和乙腈),采用电喷雾离子源负离子模式检测,外标法定量。结果:米酵菌酸在1.00~50.00 ng/mL浓度范围内线性良好,相关系数为0.99996;在优化的固相萃取法下,方法检出限为0.03μg/kg,定量限为0.1μg/kg。按低、中、高3个水平加标,回收率为97.0%~102.1%,相对标准偏差1.4%~2.7%。结论:该方法灵敏高、准确度好,能满足广西生榨米粉中米酵菌酸的测定要求。经抽样检测的结果表明,广西生榨米粉被米酵菌酸污染的风险较低。

Objective:A method for the determination of bongkrekic acid in fresh rice noodles of Guangxi Province was established by using mixed-mode anion exchange solid phase extraction combined with ultra performance liquid chromatograghy-tandem mass spectrometry(UPLC-MS).And the risk of fresh rice noodles contaminated by bongkrekic acid was preliminarily assessed.Methods:Fresh rice noodles of Guangxi Province were taken as the research objects.Mixed-mode anion exchange columns were applied to purify the target compound.The 0.1%formic acid water and acetonitrile were used as mobile phase for gradient elution.Electrospray ion source negative mode and external standard method were applied to detect the samples.Results:Bongkrekic acid showed good linear relationship in the concentration range of 1.00–50.00 ng/mL,and the correlation coefficient was 0.99996.Via the optimized solid phase extraction,the limit of detection was 0.03μg/kg,and the limit of quantification was 0.1μg/kg.Three adding levels(low,medium,high)were carried out,and the recovery rate,were 97.0%–102.1%,and the relative standard deviations were 1.4%–2.7%.Conclusion:The method showed high sensibility and good accuracy,which could meet the needs of the determination of bongkrekic acid in Guangxi fresh rice noodles.The results of sampling tests indicated that the risk of fresh rice noodles contaminated by bongkrekic acid was low.