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建立了气相色谱串联质谱(G C-M S)准确、快速测定香精香料中仲丁醇、富马酸二甲酯、咪唑和芝麻酚的分析方法。样品经甲醇超声提取15min后,通过Agilent DB-WAX(0.25mm×30m×0.25Lm)色谱柱分离,质谱进行定性,外标法对于4种目标物质进行定量分析。实验结果表明,在0.5—20mg/L的范围内,4种物质具有较好的线性,各待测物质的线性相关系数均大于0.9990,检出限为0.02—0.12mg/L,在1,5mg/L和10mg/L 3个加标水平条件下,4种禁限用物质的平均回收率为88.0%—113.1%,相对标准偏差为0.32%—6.53%。该方法前处理简单,灵敏度高,线性相关性好,重复性佳,可以满足香精香料中4种物质的同时检测。
A method for the accurate and rapid determination of sec-butanol, dimethyl fumarate, imidazole and sesamol in flavors and fragrances by gas chromatography-tandem mass spectrometry (G C-M S) has been established. The samples were extracted with methanol for 15 min and separated by Agilent DB-WAX (0.25 mm × 30 m × 0.25 Lm) column. Qualitative analysis was carried out by mass spectrometry. Quantitative analysis was performed on the four target substances by external standard method. The experimental results showed that in the range of 0.5-20mg / L, the four substances had good linearity, and the linear correlation coefficients of all the tested substances were greater than 0.9990 with the detection limits of 0.02-0.12mg / L, Under the three spiked levels of 10 mg / L and 10 mg / L, the average recoveries of the four banned substances were 88.0% -113.1% with relative standard deviations of 0.32% -6.53%. The method has the advantages of simple pretreatment, high sensitivity, good linear correlation and good repeatability, and can meet the simultaneous detection of four substances in flavor and fragrance.