气相色谱-质谱联用法测定日用品及食品中9种凉味剂的含量

Determination of Nine Kinds of Cooling Agents in Daily Necessities and Foods by Gas Chromatography-Mass Spectrometry

建立了日用品及食品中薄荷脑等9种新型凉味剂含量的测定方法。样品经乙醇超声提取后,用DB-1701MS毛细管色谱柱（30 m×0.25 mm×0.25μm）分离,选择离子监测模式（SIM）进行质谱检测。在优化分析条件下,9种凉味剂分离良好,其在0.25～250μg/m L浓度范围内线性关系良好,相关系数均大于0.996,除薄荷氧基-1,2丙二醇（0.26μg/g）外,其余凉味剂的检出限均小于0.1μg/g;在3个不同加标浓度下的平均回收率为82.8%～103.5%,相对标准偏差（RSD,n=6）均不高于3.7%。该方法灵敏、准确、可靠,能较好地分离薄荷脑等9种凉味剂,具有分析时间短、抗干扰性好、定量准确等优点,可为含薄荷（清凉）口味食品的质量控制及未知凉味剂含量样品的分析提供科学数据。

A capillary GC - MS method was established for the determination of nine kinds of new cooling agents in mint flavor foods and daily necessities. The samples were ultrasonically extracted with ethanol, and separated on a DB - 1701MS column（30 m ×0. 25 mm ×0.25μm）, then the ex- tract was detected by MS under SIM mode. Those new cooling agents have good resolution and linear relationships within the concentration range of 0.25 -250 μg/mL under the optimum conditions. The detection limits for most of cooling agents were less than 0. 1 μg/g, except menthoxypropanediol （0.26 μg/g）. The spiked recoveries were in the range of 82.8% - 103.5% with relative standard deviations（RSDs, n = 6） not more than 3.7%. The method has the advantages of short peak reten- tion, high sensitivity, accurancy, reliability, good reproducibility and selectivity, and could pro- vide some scientific data for the quality control of mint flavor food and the analysis of cooling agent composition in unknown sample.