Chengdu Institute of Food Inspection, Chengdu 611130, China.
Key Laboratory of Chemical Metrology and Applications on Nutrition and Health, State Administration for Market Regulation, Beijing 100029, China.
Anal Methods. 2024 Sep 19;16(36):6210-6219. doi: 10.1039/d4ay01132e.
Exploring and accurately detecting new adulteration markers in sesame oil is an important measure for sesame oil adulteration monitoring. In this study, two endogenous flavors sulfurol and γ-nonalactone which can be used as potential adulteration markers were first discovered in sesame oil and accurately quantified. First, the two endogenous flavors were discovered using gas chromatography-mass spectrometry (GC-MS), and their structures were confirmed by comparing the mass spectrograms with the NIST spectral library. Then the liquid chromatography-tandem mass spectrometry (LC-MS/MS) method using direct methanol extraction pretreatment and vanillin-D3 as an internal standard was developed for rapid quantitation and application. The method was successfully validated with recoveries ranging from 88.5% to 102.2% and relative standard deviations between 2.6% and 10.5% ( = 6). The combined method of GC-MS and LC-MS/MS was indicated to be efficient and highly sensitive for detection of sulfurol and γ-nonalactone in edible oil. Subsequently, 31 sesame oils from the market were detected, revealing that 31 samples contained the identified flavors within a relatively consistent range. However, the concentration of these flavor substances in one sample was abnormally high, indicating that there was a potential risk of adulteration. Therefore, the developed method shows good potential for quality evaluation and adulteration screening of sesame oil.
探索和准确检测芝麻油中的新掺伪标志物是芝麻油掺伪监测的重要措施。在本研究中,首次发现了两种内源性风味物质——亚硫酸丙烯酯和γ-壬内酯,可以作为潜在的掺伪标志物,并对其进行了准确的定量分析。首先,使用气相色谱-质谱联用技术(GC-MS)发现了这两种内源性风味物质,并通过将质谱图与 NIST 谱库进行比较,确定了它们的结构。然后,建立了一种基于直接甲醇提取预处理和香草醛-D3 内标物的液相色谱-串联质谱(LC-MS/MS)方法,用于快速定量和应用。该方法的回收率在 88.5%至 102.2%之间,相对标准偏差在 2.6%至 10.5%(n=6)之间,验证结果良好。GC-MS 和 LC-MS/MS 联合方法对于检测食用油脂中的亚硫酸丙烯酯和γ-壬内酯具有高效、高灵敏度的特点。随后,对市场上的 31 种芝麻油进行了检测,结果表明,31 个样品均含有鉴定出的风味物质,但在一个样品中这些风味物质的浓度异常高,表明存在潜在的掺伪风险。因此,所建立的方法在芝麻油的质量评价和掺伪筛选方面具有良好的应用前景。