超高效液相色谱-串联质谱法测定柳州螺蛳粉中米酵菌酸

Determination of bongkrekic acid in Liuzhou river snails rice noodle by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  柳州螺蛳粉  米酵菌酸  固相萃取

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  Liuzhou river snails rice noodle  bongkrekic acid  solid phase extraction

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定柳州螺蛳粉中米酵菌酸的分析方法。方法 样品经75%甲醇超声提取, MAX固相萃取柱净化后, 经Eclipse Plus C18 RRHD(2.1 mm×50 mm, 1.8 μm)色谱柱分离, 以乙腈和含0.1%甲酸的10 mmol/L甲酸铵溶液为流动相进行梯度洗脱, 采用ESI离子源负离子模式电离, 多反应监测模式检测。结果 米酵菌酸在1.050～1050 ng/mL浓度范围内呈良好线性关系, 方法检出限为0.01 μg/kg, 定量限为0.03 μg/kg, 平均回收率为80.4%～96.3%,相对标准偏差为1.3%~4.4%。结论 建立的测定方法简易、灵敏、准确, 可作为柳州螺蛳粉中米酵菌酸的测定方法。

英文摘要:

      Objective To establish a method for the determination of bongkrekic acid in Liuzhou river snails rice noodle by ultra performance liquid chromatography-tandem mass spectrometry. Methods After ultrasonic extraction with 75% methanol and purification with MAX solid phase extraction column, the samples were separated with Eclipse Plus C18 RRHD(2.1 mm×50 mm,1.8 μm) column by gradient elution using acetonitrile and 10 mmol/L ammonium formate solution as mobile phase, ionized by the negative ion mode of ESI ion source, and detected by the multi-reaction monitoring mode. Results Bongkrekic acid had a good linear relationship in the concentration range of 1.050–1050 ng/mL. The limit of detection was 0.01 μg/kg and the limit of quantification was 0.03 μg/kg. The average recovery rates were 80.4%–96.3%, and the relative standard deviations were 1.3%–4.4%. Conclusion The established method is simple, sensitive and accurate, and can be used as a method for determination of bongkrekic acid in Liuzhou snail rice noodle.