气相色谱- 串联质谱法测定食品中的富马酸二甲酯

为解决样品基体成分复杂、干扰测定的难题，建立一种基于气相色谱- 串联质谱(GC-MS/MS)检测食品中富马酸二甲酯的方法。通过对提取液、固相萃取柱、电离电压的考察，最终确定食品中富马酸二甲酯经乙腈提取、C18 小柱净化、CID 电压15V 最优条件。本方法在0.045～10.00mg/L 质量浓度范围内呈线性关系，相关系数为0.9998，仪器定量检出限LOQ 为0.045mg/L，外标法定量。在0.05、0.50、1.00mg/kg 3 个水平的回收相对标准偏差为2.77%～8.70%，回收率87%～108%。结果表明，相对于GC、GC-MS 方法，GC-MS/MS 方法分析时间短、无杂质峰干扰、灵敏度高，可以满足食品中检测的要求。

Gas Chromatography Couple to Tandem Mass Spectrometric Determination of Dimethyl Fumarate in Foods

To solve the problems of complexity of sample matrix and interference, gas chromatography couple with tandem mass spectrometry (GC-MS/MS) was utilized to set up a method for the determination of dimethyl fumarate in foods. Sample pretreatment prior to the injection into the instrument was achieved through extraction with acetonitrile extraction and subsequent cleanup on C18 column. The collision induced dissociation (CID) voltage selected was 15 V. The method showed good linearity over the range of 0.05 to 10.00 mg/L (R 2= 0.9998), with a limit of detection (LOQ) of 0.045 mg/L. The external standard method was used for quantification. The spike recoveries of dimethyl fumarate at spike levels of 0.05, 0.50 and 1.00 mg/kg was between 87% and 108%, with a relative standard deviation ranging from 2.77% to 8.70%. Compared with GC and GC-MS methods, the proposed GC-MS/MS method has the benefits of less time consumption and interference and higher sensitivity, and is more suitable for the analysis of foods samples in batches.