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食品与发酵工业  2019, Vol. 45 Issue (10): 182-187    DOI: 10.13995/j.cnki.11-1802/ts.018940
  分析与检测 本期目录 | 过刊浏览 | 高级检索 |
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
杨朝霞1,2*, 李梅1,2, 盛贤斌2, 董建军1,2
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)
Simultaneous determination of humuliones, hulupones, and iso-α-acids in beer by high performance liquid chromatography
YANG Zhaoxia1,2*, LI Mei1,2, SHENG Xianbin2, DONG Jianjun1,2
1(State Key Laboratory of Biological Fermentation Engineering of Beer, Qingdao 266061, China)
2(Tsingtao Brewery Co.Ltd., Qingdao 266061, China)
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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C18 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。
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杨朝霞
李梅
盛贤斌
董建军
关键词:  啤酒  苦味  葎草灵酮  希鲁酮  异α-酸  高效液相色谱    
Abstract: 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. C18 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.
Key words:  beer    bitterness    humuliones    hulupones    iso-α-acids    high performance liquid chromatography
收稿日期:  2018-09-29                出版日期:  2019-05-25      发布日期:  2019-06-17      期的出版日期:  2019-05-25
基金资助: 国家高技术研究发展(863)计划(2013AA102109)
作者简介:  硕士,高级工程师(本文通讯作者,E-mail:yangzx@tsingtao.com.cn)。
引用本文:    
杨朝霞,李梅,盛贤斌,等. 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[J]. 食品与发酵工业, 2019, 45(10): 182-187.
YANG Zhaoxia,LI Mei,SHENG Xianbin,et al. Simultaneous determination of humuliones, hulupones, and iso-α-acids in beer by high performance liquid chromatography[J]. Food and Fermentation Industries, 2019, 45(10): 182-187.
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http://sf1970.cnif.cn/CN/10.13995/j.cnki.11-1802/ts.018940  或          http://sf1970.cnif.cn/CN/Y2019/V45/I10/182
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