Natural Products Utilization Research Unit, Agricultural Research Service, United States Department of Agriculture, University, MS 38677, United States.
National Center for Natural Products Research, School of Pharmacy, University of Mississippi, University, MS 38677, United States.
J Chromatogr B Analyt Technol Biomed Life Sci. 2024 Jan 1;1232:123953. doi: 10.1016/j.jchromb.2023.123953. Epub 2023 Dec 8.
Peppermint essential oil (EO) has a multitude of applications, such as a fragrance in cosmetics, personal care and industrial products, or as a flavoring ingredient in food and beverages. Despite its popularity and economic significance, peppermint EO is often adulterated to reduce production costs and to increase profits. Although the ISO standard for peppermint EO exists, detecting sophisticated forms of adulteration remains challenging.The current study used conventional and chiral GC/MS analysis of volatiles compounds, and chemometric techniques to evaluate an extensive set of authentic peppermint EO (n = 22) and commercial products (n = 36) purported to contain peppermint EO. Specifically, thirty-six terpenoids were examined in each sample and compared with the ISO standard. Fifty-three percent of the selected commercial products did not meet the ISO specifications and the ratio between menthone/isomenthone was proven to be a good indicator for authentication and adulteration detection. Chiral GC/MS was further employed to measure eight terpenoids: α-pinene, β-pinene, limonene, menthol, menthone, isomenthone, pulegone, and menthyl acetate. The enantiomeric compositions of 27 commercial products were above or below the norm measured from authentic peppermint EOs. Of the 27 samples, eight met the ISO standard. A sample class prediction (SCP) model based on partial least squares-discriminant analysis (PLS-DA) of conventional GC/MS data was constructed using authentic peppermint EOs and cornmint EOs. The model can distinguish the most common types of peppermint EOs (US, India, and US/India blend) and cornmint EOs sold in the US market. After construction, the SCP model was then used to analyze commercial samples. One sample, which passed both ISO specification and chiral analysis, was identified as outlier by the SCP model. Overall, the applicability of combining both conventional and chiral GC/MS along with chemometric tools has been successfully demonstrated to address the overall quality of peppermint EOs in commerce and may help combat sophisticated adulteration.
薄荷精油(EO)有多种用途,例如在化妆品、个人护理和工业产品中用作香料,或在食品和饮料中用作调味成分。尽管薄荷精油很受欢迎且具有经济意义,但为了降低生产成本和提高利润,它经常被掺假。尽管存在薄荷精油的 ISO 标准,但检测复杂形式的掺假仍然具有挑战性。本研究使用常规和手性 GC/MS 分析挥发性化合物,以及化学计量技术来评估广泛的正宗薄荷精油(n=22)和商业产品(n=36),这些产品据称含有薄荷精油。具体来说,在每个样品中检查了三十六个萜烯,并与 ISO 标准进行了比较。53%的选定商业产品不符合 ISO 规格,并且薄荷酮/异薄荷酮的比例被证明是鉴定和检测掺假的良好指标。手性 GC/MS 进一步用于测量八种萜烯:α-蒎烯、β-蒎烯、柠檬烯、薄荷醇、薄荷酮、异薄荷酮、侧柏酮和乙酸薄荷酯。27 种商业产品的对映异构体组成高于或低于从正宗薄荷精油中测量到的标准。在 27 个样品中,有 8 个符合 ISO 标准。基于常规 GC/MS 数据的偏最小二乘判别分析(PLS-DA)构建了基于部分最小二乘判别分析(PLS-DA)的样品分类预测(SCP)模型,使用正宗薄荷精油和留兰香精油。该模型可以区分美国、印度和美国/印度混合最常见类型的薄荷精油和在美国市场上销售的留兰香精油。模型构建后,使用 SCP 模型分析商业样品。一个通过 ISO 规格和手性分析的样品被 SCP 模型识别为异常值。总体而言,成功证明了结合常规和手性 GC/MS 以及化学计量工具的适用性,以解决商业中薄荷精油的整体质量问题,并可能有助于打击复杂的掺假。