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目的建立液液萃取结合气相色谱/质谱法测定糕点中富马酸二甲酯(dimethyl fumarate,DMF)的方法。方法取5g捣碎样品加入25ml乙腈,超声提取10min,过滤,取2.0ml滤液加入2ml正己烷,振摇1min除脂,3000r/min离心2min,取下层有机相1μl进样分析。以DB-5色谱柱(30 m×0.25 mm,0.25μm)为分离柱,柱温采取程序升温,分流进样,分流比为1∶10。质谱测定以扫描(scan)模式定性,选择离子监测(selected ions monitoring,SIM)模式定量。结果DMF在0.010~1.0μg/m L范围内线性良好(相关系数>0.999 8),检出限为0.015μg/g。方法用于糕点的测定,加标回收率为88.0%-116%,低浓度和高浓度加标样测定值的相对标准偏差(relative standard derivation,RSD)分别为6.52%和3.60%。结论方法灵敏快速,适用于糕点中DMF的检测。随机调查了成都市各品牌糕点,均未检出DMF。
Objective To establish a liquid-liquid extraction coupled with gas chromatography / mass spectrometry for the determination of dimethyl fumarate (DMF) in cakes. Methods 5g mashed samples were added 25ml of acetonitrile, ultrasonic extraction 10min, filtered, take 2.0ml filtrate added 2ml n-hexane, shaken 1min degrease, 3000r / min centrifugation 2min, take the lower organic phase 1μl injection analysis. A DB-5 column (30 m × 0.25 mm, 0.25 μm) was used as the separation column. The temperature of the column was programmed and the split injection was performed at a split ratio of 1:10. Mass spectrometry is characterized by a scan mode, selected ion monitoring (SIM) mode. Results The linearity of DMF in the range of 0.010-1.0 μg / mL was good (correlation coefficient> 0.999 8). The detection limit was 0.015 μg / g. The method was applied to the determination of cakes with the recoveries of 88.0% -116%. The relative standard derivations (RSDs) of low and high spiked samples were 6.52% and 3.60%, respectively. Conclusion The method is sensitive and rapid and suitable for the detection of DMF in cakes. Random survey of Chengdu brand pastries, were not detected DMF.