高效液相色谱法同时检测啤酒中的葎草灵酮、希鲁酮和异α-酸  

Simultaneous determination of humuliones,hulupones,and iso-α-acids in beer by high performance liquid chromatography

作　　者：杨朝霞 李梅 盛贤斌 董建军 YANG Zhaoxia;LI Mei;SHENG Xianbin;DONG Jianjun(State Key Laboratory of Biological Fermentation Engineering of Beer,Qingdao 266061,China;Tsingtao Brewery Co.Ltd.,Qingdao 266061,China)

机构地区：[1]啤酒生物发酵工程国家重点实验室,山东青岛266061 [2]青岛啤酒股份有限公司,山东青岛266061

出　　处：《食品与发酵工业》2019年第10期182-187,共6页Food and Fermentation Industries

基　　金：国家高技术研究发展(863)计划(2013AA102109)

摘　　要：为研究啤酒苦味物质组成,利用高效液相色谱法(high performance liquid chromatography,HPLC)建立了啤酒中的葎草灵酮、希鲁酮和异α-酸的检测新技术。以高甲酸颗粒酒花为原料,60 ℃高温空气氧化后,采用Alltima C18 色谱柱分离,以体积分数为0.05%的磷酸和乙腈为流动相梯度洗脱,结合色谱图和紫外光谱特性得到葎草灵酮和希鲁酮的参考标样;用C 18 固相萃取柱(solid-phase extraction, SPE)进行样品前处理。该方法的相对标准偏差2.18%~3.59%;葎草灵酮、希鲁酮和异α-酸的最小检出限分别为0.03、0.03和0.05 mg/L;回收率95%~ 115%。分析了市售不同品类啤酒中苦味物质组成,淡色Lager、皮尔森、小麦啤酒和黑啤酒中,葎草灵酮和希鲁酮含量均不高(<2 mg/L);而IPA啤酒中葎草灵酮、希鲁酮和异α-酸含量较高,且不同品牌苦味物质组成存在较大差异。该方法为后续开展葎草灵酮、希鲁酮的苦感研究及IPA啤酒苦味物质调控提供了有效的检测手段。In order to study the composition of bitter substances in beer, high performance liquid chromatography was applied to quantitatively determine humuliones, hulupones, and iso-α-acid in beer. By oxidizing hop pellets at 60 ℃, humuliones and hulupones as major products were separated using Alltima C18 column, and 0.05% phosphoric acid and acetonitrile were used for mobile phase gradient elution. C 18 solid-phase extraction (SPE) tubes were used for sample pretreatment. The relative standard deviations (RSDs) were 2.18%-3.59%. The minimum detection limits for humuliones, hulupones, and iso-α-acid were 0.03, 0.03, and 0.05 mg/L, respectively, and their recoveries were in a range of 95%-115%. It was found that most commercial beers, such as lager beer, pilsner, wheat beer and stout, contained less humuliones and hulupones (<2 mg/L), however, India Pale Ale (IPA) had higher levels and their composition varied significantly among different brands. In conclusion, this method is effective for conducting further studies on bitter senses of humuliones and hulupones, and also for regulating bitter substances in IPA.

关 键 词：啤酒 苦味 葎草灵酮 希鲁酮 异Α-酸 高效液相色谱 

分 类 号：O657.72[理学—分析化学] TS262.5[理学—化学]