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目的建立快速测定橙汁中桔霉素的液相色谱/四极杆飞行时间质谱方法。方法采用QuEChERS法提取净化样品,外标法定量,液相色谱/四极杆飞行时间质谱法检测。结果桔霉素在0.005~0.2 mg/L浓度范围内有良好的线性(r>0.9997)。在3个不同添加水平下,样品的加标回收率范围为82.62%~104.13%,相对标准偏差(RSD)<3%。将本方法用于实际样品分析,20份市售橙汁产品中有4份检测到桔霉素。结论 QuEChERS结合液相色谱/四极杆飞行时间质谱检测方法简便快速,可用于测定橙汁中的桔霉素。
Objective To establish a liquid chromatography / quadrupole time-of-flight mass spectrometry method for rapid determination of citrinin in orange juice. Methods Purified samples were extracted by QuEChERS method and quantified by external standard method and detected by liquid chromatography / quadrupole time-of-flight mass spectrometry. Results There was a good linearity (r> 0.9997) for citrinin within the range of 0.005-0.2 mg / L. The recoveries ranged from 82.62% to 104.13% with relative standard deviations (RSDs) <3% at three different loading levels. Using this method for actual sample analysis, 4 out of 20 commercially available orange juice products detected citrinin. Conclusion QuEChERS combined LC / quadrupole time-of-flight mass spectrometry is simple and fast and can be used to determine citrinin in orange juice.