Abstract In recent years, hop aroma emerged as a key quality characteristic of popular beer styles. Accordingly, the instrumental analysis of hop derived odorants in beer advanced as a must have analytical technique for research and quality control purposes. Still, the analysis of hop aroma compounds is challenging. Substance concentrations might strongly vary depending on the beer style, matrix effects might hinder reliable quantification, and SPME-GC-MS based protocols are suspected to lack (long-term) stability. The current paper describes the validation and application of a headspace solid-phase microextraction (HS-SPME) – gas chromatography (GC) – tandem mass spectrometry (MS/MS) method for analysis of 16 selected hop aroma compounds in beer. To enable rapid and reliable quantification of selected terpenes, terpenoids, and esters across a wide working range (1–1000 µg/L), instrumental parameters were optimized and three stable isotope labeled standards, namely d5-linalool, d2-myrcene, and d6-citronellol were synthesized and characterized by nuclear magnetic resonance (NMR) spectroscopy. Extensive method validation and routine application proves the excellent selectivity, sensitivity, and robustness of the method in all relevant matrices such as light hopped lagers and dry-hopped ales.

中文翻译：

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使用 HS-SPME-GC-MS/MS 分析商业拉格啤酒和精酿啤酒中选定的啤酒花香气化合物

摘要 近年来，啤酒花香气已成为流行啤酒风格的关键品质特征。因此，啤酒中啤酒花衍生气味的仪器分析已成为研究和质量控制目的的必备分析技术。尽管如此，啤酒花香气化合物的分析仍然具有挑战性。物质浓度可能会因啤酒风格而有很大差异，基质效应可能会阻碍可靠的量化，并且怀疑基于 SPME-GC-MS 的协议缺乏（长期）稳定性。本论文描述了顶空固相微萃取 (HS-SPME) - 气相色谱 (GC) - 串联质谱 (MS/MS) 方法的验证和应用，用于分析啤酒中 16 种选定的啤酒花香气化合物。为了能够快速可靠地定量选定的萜烯、萜类化合物、和酯在很宽的工作范围内 (1–1000 µg/L)，优化了仪器参数，合成了三种稳定同位素标记的标准品，即 d5-芳樟醇、d2-月桂烯和 d6-香茅醇，并通过核磁共振 (NMR) 进行表征) 光谱学。广泛的方法验证和常规应用证明了该方法在所有相关基质（例如淡啤酒啤酒和干啤酒啤酒）中具有出色的选择性、灵敏度和稳定性。