超高效液相色谱-串联质谱法测定米粉和 河粉中的米酵菌酸

Determination of bongkrekic acid in rice noodles and fried rice noodles by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  米酵菌酸  液相色谱-串联质谱法  米粉  河粉

英文关键词:bongkrekic acid  ultra performance liquid chromatography-tandem mass spectrometry  rice noodles  fried rice noodles

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定河粉和米粉中米酵菌酸(bongkrekic acid, BA)的含量。方法 试样经提取、净化、浓缩及过滤后, 以0.1%甲酸水和乙腈作为流动相进行梯度洗脱, 采用电喷雾离子源负模式检测, 外标法定量。基于米酵菌酸色谱和质谱行为的研究, 对其仪器测定条件进行优化, 并对优化后的方法进行方法学验证。结果 米酵菌酸在1~100 μg/L浓度范围内线性良好, 相关系数大于0.999。在2种基质不同加标浓度下, 回收率80.6%~104.8%, 相对标准偏差小于5%。米酵菌酸在2种基质中的检出限为0.1 μg/kg, 定量限为0.2 μg/kg。结论 方法灵敏度高、专属性好、准确可靠, 适用于米粉和河粉基质中米酵菌酸的测定。

英文摘要:

      Objective To establish a method for the determination of bongkrekic acid (BA) in rice noodles and fried rice noodles by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After the samples were extracted, purified, concentrated and filtered, 0.1% formic acid water and acetonitrile were used as mobile phase for gradient elution. The samples were detected by electrospray ion source negative mode (ESI-) and quantified by external standard method. Based on the study of the chromatographic and mass spectrometric behaviors of BA, the conditions of its instrumental determination were optimized, and the optimized method was validated. Results BA had a good linearity in the concentration range of 1100 μg/L, and the correlation coefficient was greater than 0.999. Under the different spiked concentrations of two substrates, the recoveries were 80.6%104.8%, with the relative standard deviations were less than 5%. The limits of detection of 2 matrices were 0.1 μg/kg, and the limits of quantification were 0.2 μg/kg. Conclusion This method has high sensitivity, good specificity, accuracy and reliability, which is suitable for the determination of BA in rice noodles and fried rice noodles .