首页|UPLC-MS/MS同时检测湿米粉(粉条)中脱氢乙酸、米酵菌酸

UPLC-MS/MS同时检测湿米粉(粉条)中脱氢乙酸、米酵菌酸

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建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时检测湿米粉(粉条)中脱氢乙酸、米酵菌酸的方法.样品经0.2%氨水-80%甲醇水溶液提取,上清液过0.22 μm微孔滤膜,经Agilent InfinityLab Poroshell 120 EC-C18柱(2.1 mm × 50 mm,1.9 μm)分离,以5 mmol/L乙酸铵(氨水调节pH 8.0)-甲醇为流动相,采用电喷雾离子源(electrospray ionization,ESI)负离子多反应监测模式检测,外标法定量.结果表明,在优化后的条件下,脱氢乙酸、米酵菌酸分别在1~100 mg/L、1~100 μg/L范围内线性关系良好,线性相关系数大于0.999,方法检出限分别为0.092 mg/kg、1.8 μg/kg.脱氢乙酸在加标水平分别为4.0,20.0和80.0mg/kg情况下,回收率为88.0%~99.8%,相对标准偏差(n=6)为1.0%~3.4%.米酵菌酸加标水平分别为8.0,100和240 μg/kg情况下,回收率为89.8%~106.1%,相对标准偏差(n=6)为1.4%~2.5%.该方法简便快捷、重复性好、灵敏度高、准确性高,可同时检测湿米粉(粉条)的脱氢乙酸、米酵菌酸.
Simultaneous Determination of Dehydroacetic Acid and Bongkrekic Acid in Wet Rice Noodles and Wet Vermicelli by UPLC-MS/MS
Establish a method for simultaneous determination of dehydroacetic acid and bongkrekic acid in wet rice noodles and wet vermicelli by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).After the samples are extracted with 0.2%ammonia-80%methanol solution,the supernatant is obtained and passed through 0.22 μm microporous membrane,then separated with Agilent Infinity Lab Poroshell 120 EC-C18 column(2.1 mm×50 mm,1.9 μm),using 5 mmol/L ammonium acetate and methanol as mobile phase,detected by the electrospray ionization(ESI)negative ion multiple reaction monitoring mode,and quantified by external standard method.The results show that under optimized condition,dehydroacetic acid and bongkrekic acid have a good linear relationship in the range of 1-100 mg/L and 1-100 μg/L,respectively,and the detection limits of the method are 0.092 mg/kg and 1.8 μg/kg,respectively.The recovery rates of dehydroacetic acid at spiked levels of 4.0,20.0,and 80.0 mg/kg are 88.0%-99.8%,and the relative standard deviation(n=6)is 1.0%-3.4%.The recovery rates of bongkrekic acid at spiked levels of 8.0,100,and 240 μg/kg are 89.8%-106.1%,and the relative standard deviation(n=6)is 1.4%-2.5%.This method is simple,rapid,convenient,repeatable,sensitive and accurate,and can simultaneously detect dehydroacetic acid and bongkrekic acid in wet rice noodles and wet vermicelli.

ultra-performance liquid chromatography-tandem mass spectrometrydehydroacetic acidbongkrekic acidwet rice noodleswet vermicelli

周海青、黄素美

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河源市疾病预防控制中心(河源 517000)

超高效液相色谱-串联质谱法 脱氢乙酸 米酵菌酸 湿米粉 湿粉条

2024

食品工业
上海市食品工业研究所

食品工业

影响因子:0.47
ISSN:1004-471X
年,卷(期):2024.45(4)
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