凝胶渗透色谱净化-气相色谱-质谱-内标法 测定焙烤食品中富马酸二甲酯

Determination of dimethyl fumarate in bakery food by gel permeation chro-matography-gas chromatography-mass spectrometry with internal standard

中文关键词:  内标  凝胶渗透色谱法  气相色谱质谱法  富马酸二甲酯  焙烤食品

英文关键词:internal standard  gel permeation chromatography  gas chromatography-mass spectrometry  dimethyl fumarate  bakery food

中文摘要:

      目的 建立凝胶渗透色谱净化-气相色谱-质谱-内标法测定焙烤食品中富马酸二甲酯残留量的方法。 方法 试样经乙酸乙酯超声提取, 经凝胶渗透色谱(gel permeation chromatography, GPC)净化, 采用选择离子监测模式(selective ion monitoring, SIM)进行气相色谱-质谱(gas chromatography-mass spectrometry, GC-MS)测定, 采用丁二酸二甲酯作为内标, 以内标法定量。结果 富马酸二甲酯在0.02~5.00 mg/L 内呈良好的线性关系, 相关系数(r)大于0.9999; 0.1、0.2和1.0 mg/kg水平的空白糕点加标回收实验的回收率为92.0%~107 %, 相对标准偏差(RSD)为3.2%~5.7 % (n=6); 方法的检出限(limit of detection, LOD)为0.012 mg/kg, 定量限(limit of quantity, LOQ)为0.04 mg/kg。结论 该方法准确、灵敏度高, 适用于糕点等焙烤食品中富马酸二甲酯残留水平测定。

英文摘要:

      To determine dimethyl fumarate in bakery food by gel permeation chromatography (GPC) -gas chromatography-mass spectrometry (GC-MS) with internal standard calibration. Methods Samples with dimethyl succinate as internal standard were ultrasonically extracted by ethyl acetate, and followed by GPC clean up to remove fat and oils. Dimethyl fumarate was quantified by GC-MS under selected ion moni-toring (SIM) mode. Results Dimethyl fumarate showed a linearity in the range of 0.02~5.00 mg/L with the correlation coefficients not less than 0.9999. The relative recoveries of the spiked blank cake samples were in the range of 92.0%~107% with the relative standard deviations (RSD) in the range of 3.2%~5.7% (n=6). The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.012 mg/kg and 0.04 mg/kg, respectively. Conclusion The established method is accurate and sensitive, and suitable to determine dimethyl succinate residue in bakery samples.