对大米中四种香精采用高效液相色谱-四极杆/静电场轨道阱高分辨率质谱建立了检测方法。大米样品 经水溶液浸泡，加入酸化的乙腈提取、涡旋震荡12 min、离心后，提取液过C18固相萃取柱，流出液过0.45 μm滤膜。梯度洗脱采用乙腈-0.1%（V/V）甲酸水溶液为流动相，分析色谱柱采用Agilent EclipsePlus C18（100 mm×2.1 mm，1.8 μm）。质谱采用正离子模式，采用Full MS/dd-MS2扫描模式，以一级质谱提取的母离子对应峰面积进行定量，以自动触发扫描所得的二级子离子进行定性确证，外标法定量。四种香精香兰素、甲基香兰素、乙基香兰素、香豆素在所建立的色谱条件下分离度较好。该方法对四种香精的检测限可达15 μg/kg，定量限可达50 μg/kg，在5~500 ng/mL质量浓度范围内线性关系良好，相关系数均大于0.99。在三个浓度水平下进行加标验证，四种香精的平均回收率为79.0%~95.8%、相对标准偏差（RSD）为3.1%~7.7%。该方法样品处理过程简单，回收率高、稳定性好，可以用于大米中四种香精的筛查和确证，为规范大米中香精的使用具有重要意义。

A method for determining four flavor compounds in rices by high-performance liquid chromatographyquadrurpole/electrostatic field orbitrap high-resolution mass spectrometry (HPLC-Q/Qrbitrap MS) was developed. The rice samples were soaked in a water solution, extracted by acidified acetonitrile, vortexed via oscillation for 12 min, and then centrifuged, the extract passed through a C18 solid-phase extraction column, and the effluent passed through a 0.45 μm filter membrane. The gradient elution was carried out with acetonitrile -0.1% (V/V) formic acid solution as the mobile phase, and Agilent EclipsePlus C18 (100 mm×2.1 mm, 1.8 μm) was used as the chromatographic column. The positive ion mode and Full MS/dd-MS2 scanning mode were used in the mass spectrometry. The corresponding peak area of parent ions extracted from the first-order mass spectrometry was quantified, and the secondary ions obtained by automatic trigger scanning were qualitatively confirmed. The samples were analyzed based on the external standard method. Under the established chromatographic conditions, four flavor compounds were well separated. The detection limits and quantification limits were 15 μg/kg and 50 μg/kg, respectively. Good linearity was obtained in the range of 5~500 ng/mL, and the correlation coefficients were all higher than 0.99. The average recoveries at three concentration levels were in the range of 79.0%~95.8% and the relative standard deviations (RSDs) were in the range of 3.1%~7.7%. The proposed method requires a simple sample treatment, and results in a high recovery rate and high stability. Therefore, can be used to screen and confirm four rice flavors, which is of great significance for regulation the application of the flavors in rice.

海关总署课题-针对境内外法规差异性食品添加剂的快速筛查（2021HK192）