超声辅助液液萃取-超高效液相色谱-串联质谱法测定米粉、河粉中的米酵菌酸

Determination of bongkrekic acid in rice noodles and chow fun by ultra performance liquid chromatography-tandem mass spectrometry with ultrasonic assisted liquid-liquid extraction

中文关键词:  超声辅助  液液萃取  超高效液相色谱-串联质谱法  米酵菌酸  米粉  河粉

英文关键词:ultrasonic assisted  liquid-liquid extraction  ultra performance liquid chromatography-tandem mass spectrometry  bongkrekic acid  rice noodles  chow fun

中文摘要:

      目的 建立超声辅助液液萃取-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)快速测定米粉、河粉中米酵菌酸(bongkrekic acid, BA)的方法。方法 称取适量已匀浆好的样品, 加入乙腈超声提取、离心后取上清液, 过0.22 μm的微孔滤膜, 经Thermo Hypersil GOLD C18柱(2.1 mm×100 mm, 1.9 μm)分离, 以0.2%甲酸-乙腈为流动相。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 在优化的条件下, 米酵菌酸在0.5~100 ng/mL范围内线性关系良好, 相关系数大于0.999, 米粉和河粉中米酵菌酸的检出限均为为0.01 μg/kg, 定量限均为0.03 μg/kg, 样品加标回收率为81.0%~90.4%, 相对标准偏差≤5.5%。结论 该方法快速、灵敏、准确, 可应用于米粉、河粉中的米酵菌酸的测定。

英文摘要:

      Objective To establish a method for the determination of bongkrekic acid (BA) in rice noodles and chow fun by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with ultrasonic assisted liquid-liquid extraction. Methods The homogenized sample were weighed a proper amount. After ultrasonic extraction with acetonitrile and centrifugation, the supernatant was obtained and passed through 0.22 μm microporous membrane, then separated with Thermo Hypersil GOLD C18 column (2.1 mm×100 mm, 1.9 μm) using 0.2% formic acid and acetonitrile as mobile phase, detected by the electrospray ionization (ESI) negative ion multiple reaction monitoring mode, and quantified by external standard method. Results Under the optimized conditions, bongkrekic acid had a good linear relationship in the range of 0.5-100 ng/mL, and the correlation coefficient was greater than 0.999. The limits of detection of bongkrekic acid in rice noodles and chow fun were 0.01 μg/kg and the limits of quantitation were 0.03 μg/kg. The average recoveries for bongkrekic acid were 81.0%-90.4% with relative standard deviations no more than 5.5%. Conclusion The proposed method is rapid, sensitive and accurate, which is suitable for the determination of bongkrekic acid in rice noodles and chow fun samples.