QuEChERS净化结合超高效液相色谱-串联质谱法快速检测汉中面皮中米酵菌酸含量

Determination of bongkrekic acid content in Hanzhong Mianpi by ultra performance liquid chromatography-tandem mass spectrometry combined with QuEChERS purification

中文关键词:  超高效液相色谱-串联质谱法  QuEChERS净化  米酵菌酸  汉中面皮

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  QuEChERS purification  bongkrekic acid  Hanzhong Mianpi

中文摘要:

      目的 建立一种QuEChERS前处理净化结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)快速检测汉中面皮中米酵菌酸含量的方法。方法 面皮样品采用乙腈-水(8:2, V:V)超声提取, QuEChERS净化处理, 浓缩、定容, 选用Thermo (100 mm×2.1 mm, 1.8 μm)色谱柱分离, 以乙腈和0.1%甲酸水溶液进行梯度洗脱, 电喷雾离子源(electron spray ionization, ESI), 负离子多反应监测(multiple reaction monitoring, MRM)模式, 以标准曲线法定量。结果 米酵菌酸在1~100 ng/mL范围内线性关系良好, 相关系数(r2)大于0.999, 在2、10、50 μg/kg低中高3个加标水平下, 加标回收率为86.7%~90.0%, 相对标准偏差(relative standard deviation, RSD)为2.3%~2.9%, 检出限为0.5 μg/kg, 定量限为1.5 μg/kg。所有实际样品均未检出米酵菌酸。结论 该方法前处理简单、分析快速、回收率高、灵敏度高, 可为汉中面皮中米酵菌酸的质量控制提供参考。

英文摘要:

      Objective To establish a method for rapid determination of bongkrekic acid content in Hanzhong Mianpi by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with QuEChERS purification. Methods Hanzhong Mianpi samples were extracted by acetonitrile-water (8:2, V:V) ultrasonic extraction, purified by QuEChERS, concentrated, constant volume, separated by Thermo (100 mm× 2.1 mm, 1.8 μm) chromatographic column, gradient eluted by acetonitrile and 0.1% formic acid aqueous solution, quantified by standard curve method with electric spray ion source (ESI), multiple reaction monitoring (MRM) mode. Results The linear relationship of bongkrekic acid was good within the range of 1–100 ng/mL, with a correlation coefficient (r2) greater than 0.999. At 3 spiked levels of 2, 10 and 50 μg/kg, the spiked recovery rate was 86.7%–90.0%, the relative standard deviation (RSD) was 2.3%–2.9%, the limit of detection was 0.5 μg/kg, and the limit of quantitation was 1.5 μg/kg. All actual samples did not detect any citric acid. Conclusion This method has simple pre-treatment, fast analysis, high recovery rate, and high sensitivity, which can provide reference for the quality control of bongkrekic acid in Hanzhong Mianpi.