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通过对色谱柱、色谱条件和前处理条件的选择优化,建立了毛细管气相色谱-质谱联用法准确、快速测定香精香料中甲醇和仲丁醇的分析方法。样品经过超声萃取过滤后,再注入气相色谱-质谱联用仪进行分析,采用选择离子和保留时间定性,内标法定量。香精香料中甲醇的回收率为95.56%~100.32%,相对标准偏差(RSD)<2.0%(n=6),检出限为0.13 mg/L,定量限为0.44 mg/L;仲丁醇回收率为94.39%~103.32%,RSD<5.0%(n=6),检出限为0.03 mg/L,定量限为0.10 mg/L。该方法与企业标准YQ/T 38-2013相比,测量结果具有良好的一致性,且该方法前处理简单、快速,准确度和灵敏度高,适合大批量样品的测定。
Through the selection and optimization of chromatographic conditions, chromatographic conditions and pretreatment conditions, an analytical method was established for the accurate and rapid determination of methanol and sec-butanol in flavors and fragrances by capillary gas chromatography-mass spectrometry. After the sample was filtered by ultrasonic extraction and then injected into gas chromatography - mass spectrometry analysis, the use of selected ions and retention time qualitative, internal standard method. The recovery of methanol in flavors and fragrances was 95.56% ~ 100.32%, RSD was less than 2.0% (n = 6), the limit of detection was 0.13 mg / L and the limit of quantification was 0.44 mg / L. Rates ranged from 94.39% to 103.32% with RSD <5.0% (n = 6). The detection limit was 0.03 mg / L and the limit of quantification was 0.10 mg / L. Compared with the enterprise standard YQ / T 38-2013, this method has good consistency of measurement results. The method is simple, rapid, accurate and sensitive, and suitable for the determination of large quantities of samples.