一种快速测定糕点中富马酸二甲酯的气相色谱质谱法

发布时间：2018-08-28 08:06

【摘要】：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。
[Abstract]:Objective to establish a method for the determination of dimethyl fumarate (dimethyl fumarate,DMF) in pastry by liquid-liquid extraction and gas chromatography / mass spectrometry. Methods 25ml acetonitrile was added to 5 g mashed sample, ultrasonic extraction was carried out for 10 min, 2.0ml filtrate was added to 2ml n-hexane, shaking 1min was centrifuged for 2 min and the lower organic phase was analyzed by 1 渭 l injection. The DB-5 column (30 m 脳 0.25 mm,0.25 渭 m) was used as the separation column. The column temperature was programmed and the sample was divided into samples. The separation ratio was 1: 10. Mass spectrometry was performed by scanning (scan) mode and ion monitoring (selected ions monitoring,SIM mode was selected for quantitative analysis. Results the linear range of DMF was 0.010 渭 g / mL (correlation coefficient 0.999 8) and the detection limit was 0.015 渭 g / g. The method was applied to the determination of pastry. The recoveries were 88.0-116. The relative standard deviations (relative standard derivation,RSD) of low concentration and high concentration were 6.52% and 3.60%, respectively. Conclusion the method is sensitive, rapid and suitable for the detection of DMF in pastry. No DMF. was detected in all brands of cakes in Chengdu.
【作者单位】：四川大学华西公共卫生学院(华西第四医院);遂宁市疾病预防控制中心;
【基金】：四川大学校级创新创业项目
【分类号】：O657.63;R155.5

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