超高效液相色谱-四极杆静电场轨道阱高分辨质谱法快速筛查和确证食品中米酵菌酸

Rapid screening and confirmation of bongkrekic acid in foods by ultra performance liquid chromatography-quadrupole-orbitrap high resolution mass spectrometry

中文关键词:  米酵菌酸  超高效液相色谱-四极杆静电场轨道阱高分辨质谱法  筛查  确证

英文关键词:bongkrekic acid  ultra performance liquid chromatography-quadrupole-orbitrap high resolution mass spectrometry  screening  confirmation

中文摘要:

      目的 建立超高效液相色谱-四极杆静电场轨道阱高分辨质谱法(ultra performance liquid chromatography-quadrupole-orbitrap high resolution mass spectrometry, UPLC-Q-Orbitrap HRMS)快速筛查和确证食品(银耳、木耳、粉条)中米酵菌酸。方法 样品用水浸泡后用甲醇涡旋振荡提取、过滤后直接采用UPLC-Q-Orbitrap HRMS测定, 采用电喷雾负离子同时进行一级、二级高精度全扫描, 得到母离子和碎片离子精确质量数, 同时进行定性定量分析, 外标法定量。结果 米酵菌酸在1.0~20.0 μg/L范围内线性良好, 相关系数0.9997, 定量限(limit of quantitation, LOQ, S/N≥10)为0.05 mg/kg, 在0.05、0.10、0.25 mg/kg加标水平下, 回收率在89.0%~96.0%之间, 相对标准偏差为4.1%~9.6%。结论 该方法前处理简单、快速、准确性好, 能够满足食品中米酵菌酸的快速筛查和确证分析。

英文摘要:

      Objective To establish an ultra performance liquid chromatography coupled to quadrupole orbitrap high-resolution mass spectrometry (UPLC-Q-Orbitrap-HRMS) method for the rapid screening and confirmation of bongkrekic acid in foods (tremella, agaric and vermicelli). Methods The samples were soaked in water and extracted by methanol with vortex. After filtration, the sample extract was directly determined by UPLC-Q-Orbitrap HRMS, the primary and secondary high-precision full scanning was carried out simultaneously by electrospray negative ion, and the accurate mass numbers of parent ion and fragment ion were obtained, qualitative and quantitative analyses were carried out at the same time, and the external standard method was carried out for quantification. Results There was a good linearity for bongkrekic acid in the range of 1.0?20.0 μg/L with correlation coefficient higher than 0.9997. The limit of quantitation (LOQ, S/N≥10) of the method was 0.05 mg/kg. The average recoveries at 3 spiking levels (0.05, 0.10, 0.25 mg/kg) were 89.0%?96.0%, and the relative standard deviations (RSDs) were 4.1%?9.6%. Conclusion This method is simple, rapid and accurate, and can meet the requirements of rapid screening and confirmation of bongkrekic acid in foods.