液相色谱/四极杆飞行时间质谱法测定 橙汁中的桔霉素

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(r0.9997)。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。

Determination of citrinin in orange juice by liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry

Objective To establish a method for determination of citrinin in orange juice by liquid chro-matography-hybrid quadrupole time-of-flight mass spectrometry (LC-Q-TOF). Methods The samples were extracted by QuEChERS method, and citrinin were separated by LC-Q-TOF, then measured by external standard method. Results Citrinin standard curve had a good linearity relationship within 0.005~0.2 mg/L (r>0.9997). Average recovery rate of samples was between 82.62% and 104.13% at 3 adding levels, and RSD<3.0%. Totally 20 orange juice samples by the current method was successfully performed. The citrinin was observed in 4 samples. Conclusion The quantitative method is rapid, simple, and high sensitive, which can be applied in the accurate determination of citrinin in orange juice.