不同類型國(guó)產(chǎn)橡木制品對(duì)葡萄酒陳釀香氣的影響

李蘭曉,李記明,*,徐 巖,,范文來,唐 柯,于 英,韓 鵬,趙榮華

(1.煙臺(tái)張?jiān)＜瘓F(tuán)有限公司技術(shù)中心,山東煙臺(tái) 264000;2.江南大學(xué)生物工程學(xué)院釀酒微生物與應(yīng)用酶學(xué)實(shí)驗(yàn)室,教育部工業(yè)生物技術(shù)重點(diǎn)實(shí)驗(yàn)室，江蘇無錫 214122)

不同類型國(guó)產(chǎn)橡木制品對(duì)葡萄酒陳釀香氣的影響

李蘭曉1,李記明1,*,徐 巖1,2,范文來2,唐 柯2,于 英1,韓 鵬1,趙榮華1

(1.煙臺(tái)張?jiān)＜瘓F(tuán)有限公司技術(shù)中心,山東煙臺(tái) 264000;2.江南大學(xué)生物工程學(xué)院釀酒微生物與應(yīng)用酶學(xué)實(shí)驗(yàn)室,教育部工業(yè)生物技術(shù)重點(diǎn)實(shí)驗(yàn)室，江蘇無錫 214122)

采用頂空固相微萃取與氣相色譜-質(zhì)譜聯(lián)用技術(shù),檢測(cè)蒙古櫟制成的橡木片和橡木板陳釀的葡萄酒中主要陳釀香氣成分的變化。結(jié)果表明:在90 d的陳釀過程中,糠醛和5-甲基糠醛含量在陳釀10至20 d即可達(dá)到最高值,此后其含量快速減少;愈創(chuàng)木酚和甲基愈創(chuàng)木酚含量則在陳釀20 d達(dá)到最高值以后,基本保持不變;順式和反式橡木內(nèi)酯含量在整個(gè)陳釀過程中一直呈增加趨勢(shì);而香草醛含量在采用橡木片和橡木板陳釀的葡萄酒中,具有不同的變化趨勢(shì):橡木片陳釀的葡萄酒,香草醛含量在30d時(shí)即達(dá)到最高值,此后逐漸減少,而橡木板陳釀的葡萄酒,香草醛含量在90 d的陳釀過程中一直增加;乙基愈創(chuàng)木酚和乙基苯酚含量?jī)H在陳釀30和60 d后才顯著增加。橡木片和橡木板陳釀的葡萄酒之間,除乙基苯酚和乙基愈創(chuàng)木酚含量無顯著差異外,糠醛、香草醛、愈創(chuàng)木酚和橡木內(nèi)酯的含量均具有顯著差異,表明橡木制品的類型對(duì)葡萄酒的陳釀香氣具有重要影響。

橡木制品,葡萄酒,陳釀香氣

橡木桶陳釀是葡萄酒生產(chǎn)中的重要工藝環(huán)節(jié)。橡木桶陳釀過程中,葡萄酒發(fā)生復(fù)雜的物理、化學(xué)及生物化學(xué)變化,葡萄酒的顏色、香氣、口感均得以明顯改善,尤其是橡木中的一些揮發(fā)性香氣成分,如橡木內(nèi)酯類、酚醛類、糠醛類、揮發(fā)酚類化合物,可使葡萄酒產(chǎn)生香草、煙熏、咖啡、甘草等復(fù)雜香氣,是葡萄酒產(chǎn)生陳釀特征的主要物質(zhì)[1]。但橡木桶陳釀也有一些缺點(diǎn),如投資成本高,陳釀周期長(zhǎng),需定期更新等。因此,為了獲得類似橡木桶陳釀的效果,人們研究使用橡木制品進(jìn)行陳釀,如橡木片、橡木板等。由于價(jià)格低廉,使用方便,橡木制品在美國(guó)、澳大利亞等地得到廣泛應(yīng)用[2],尤其是2006年,歐盟對(duì)葡萄酒的法規(guī)進(jìn)行了修訂,允許在葡萄酒中使用橡木制品,進(jìn)一步促進(jìn)了對(duì)橡木制品的研究與應(yīng)用[3]。

目前,用于葡萄酒的橡木制品,主要是產(chǎn)自法國(guó)的無柄橡(Quercus petraea)和有柄橡(Quercus robur)及產(chǎn)自美國(guó)的美洲白橡(Quercus alba)。此外,為開發(fā)新的橡木資源,國(guó)外學(xué)者還對(duì)西班牙等地不同品種的橡木開展了深入研究[4-5]。我國(guó)東北長(zhǎng)白山等地具有大量橡木資源,與歐美的橡木均屬櫟屬植物,其結(jié)構(gòu)和成分與歐洲橡木相似,國(guó)內(nèi)已有多家以國(guó)產(chǎn)橡木為原料生產(chǎn)橡木制品的企業(yè),但對(duì)于國(guó)產(chǎn)橡木制品在葡萄酒中的應(yīng)用效果,尤其是國(guó)產(chǎn)橡木制品對(duì)葡萄酒中源于橡木的特征香氣成分的影響少有研究報(bào)道。因此,本研究采用我國(guó)東北地區(qū)的蒙古櫟(Quercus mongolica),分別制成中度烘烤的橡木片和橡木板,并應(yīng)用于葡萄酒陳釀,采用固相微萃取與氣質(zhì)聯(lián)用(SPME-GC-MS)的方法,對(duì)陳釀過程中葡萄酒中源于橡木的陳釀香氣成分進(jìn)行分析,以期探索采用國(guó)產(chǎn)橡木制品陳釀期間,葡萄酒主要陳釀香氣成分的變化規(guī)律,進(jìn)而為國(guó)產(chǎn)橡木制品在葡萄酒生產(chǎn)中的應(yīng)用提供理論依據(jù)。

1 材料與方法

1.1 材料與試劑

1.1.1 葡萄酒 2013年釀造的蛇龍珠葡萄酒,由煙臺(tái)張?jiān)Ｆ咸丫乒咎峁?。葡萄酒轉(zhuǎn)入200 L的不銹鋼儲(chǔ)酒罐中,分別添加橡木片和橡木板進(jìn)行陳釀。入罐時(shí),葡萄酒的主要理化指標(biāo)如下:酒精度12.0%,總酸5.4 g/L,揮發(fā)酸0.35 g/L,pH3.8,殘?zhí)?.6 g/L,總二氧化硫60 mg/L。

1.1.2 橡木板和橡木片 采用同一批次未經(jīng)烘烤的蒙古櫟(Quercus mongolica)分別制成橡木板(1000 mm×40 mm×10 mm)和橡木片(2 mm×1 mm×0.5 mm),然后在200±10 ℃的溫度條件下,烘烤30 min,用于葡萄酒的陳釀。

1.1.3 試劑 2-辛醇,糠醛,5-甲基糠醛,順式橡木內(nèi)酯,反式橡木內(nèi)酯,香草醛,愈創(chuàng)木酚,4-甲基愈創(chuàng)木酚,4-乙基愈創(chuàng)木酚,4-乙基苯酚 均購(gòu)自美國(guó)Sigma公司,純度98%以上;氯化鈉,分析純 上海國(guó)藥集團(tuán)化學(xué)試劑有限公司。

1.2 儀器與設(shè)備

Agilent氣相色譜6890-5975質(zhì)譜聯(lián)用儀 美國(guó)Agilent公司;MPS2固相微萃取自動(dòng)進(jìn)樣器 德國(guó)Gerstel公司;碳分子篩/聚二乙烯苯/聚二甲基硅氧烷(DVB/CAR/PDMS,50/30 μm)萃取頭,DB-FFAP 色譜柱(60 m×0.25 mm,0.25 μm) 美國(guó)Supelco公司。

1.3 實(shí)驗(yàn)方法

1.3.1 葡萄酒的陳釀 按照葡萄酒中橡木制品的表面積為90 cm2/L的添加量,在100 L的葡萄酒中分別添加橡木片和橡木板,室溫條件下陳釀90 d,期間分別在10、20、30、60和90 d時(shí)取樣進(jìn)行分析,每種處理均設(shè)3個(gè)平行,并以同樣條件下陳釀,但未加橡木制品的葡萄酒為對(duì)照。

1.3.2 香氣成分測(cè)定 參照文獻(xiàn)[6]所述方法,略有修改,對(duì)相關(guān)的揮發(fā)性成分進(jìn)行測(cè)定。準(zhǔn)確吸取8 mL酒樣于20 mL頂空瓶中,加入3 g NaCl,加入100 μL濃度為1 mg/L的2-辛醇作為內(nèi)標(biāo),用聚四氟乙烯隔墊密封,預(yù)平衡溫度和萃取溫度為70 ℃,預(yù)平衡時(shí)間2 min、萃取時(shí)間60 min,進(jìn)行GC-MS分析,解吸溫度250 ℃,解吸時(shí)間5 min。

色譜條件:色譜柱為DB-FFAP色譜柱(60 m×0.25 mm,0.25 μm);進(jìn)樣口溫度250 ℃;升溫程序:50 ℃保持2 min,然后以4 ℃/min升至230 ℃,保持15 min;載氣He,流速2 mL/min,不分流進(jìn)樣。

質(zhì)譜條件:質(zhì)譜接口溫度為250 ℃;離子源溫度230 ℃;電離方式EI;電子能量70 eV;質(zhì)量掃描范圍為40～500 u。

通過標(biāo)準(zhǔn)品的保留時(shí)間以及NIST 05質(zhì)譜庫(kù)(Agilent Technologies Inc.)檢索,結(jié)合文獻(xiàn)報(bào)道的保留指數(shù)進(jìn)行定性。采用內(nèi)標(biāo)標(biāo)準(zhǔn)曲線法進(jìn)行定量,每種待測(cè)物質(zhì)分別對(duì)應(yīng)于內(nèi)標(biāo)作標(biāo)準(zhǔn)曲線。樣品采用GC-MS檢測(cè),利用待測(cè)物質(zhì)和內(nèi)標(biāo)的峰面積比代入相應(yīng)的標(biāo)準(zhǔn)曲線方程計(jì)算出待測(cè)物質(zhì)的含量。

1.4 數(shù)據(jù)統(tǒng)計(jì)分析

統(tǒng)計(jì)分析采用SPSS 19.0分析軟件進(jìn)行。繪圖采用Excel。

2 結(jié)果與分析

2.1 陳釀過程中糠醛和5-甲基糠醛含量的變化

糠醛和5-甲基糠醛是橡木中纖維素和半纖維素的熱解產(chǎn)物,具有烤面包氣味,但這兩種化合物由于閾值較高,在葡萄酒中的濃度一般低于其閾值,其對(duì)葡萄酒香氣的影響,主要是通過協(xié)同效應(yīng),增強(qiáng)葡萄酒中的橡木香氣[7]。由圖1和圖2可知,采用橡木片和橡木板處理的葡萄酒在陳釀過程中,糠醛和5-甲基糠醛含量的變化趨勢(shì)基本一致,橡木片和橡木板陳釀的葡萄酒中,糠醛和5-甲基糠醛含量在10 d和20 d即達(dá)到最高值,此后其含量快速減少,至陳釀90 d時(shí),葡萄酒中糠醛和5-甲基糠醛含量?jī)H相當(dāng)于其最高值的12%～17%。但橡木板陳釀的葡萄酒中,糠醛和5-甲基糠醛含量均顯著(p<0.05)高于橡木片陳釀的葡萄酒,表明在相同烘烤程度和用量的條件下,橡木板產(chǎn)生的糠醛化合物含量更高。而在陳釀過程中,糠醛和5-甲基糠醛含量呈先上升后下降的變化趨勢(shì),可能是由于糠醛和5-甲基糠醛可參與多種化學(xué)反應(yīng)所致,例如,通過氧化還原反應(yīng)生成糠醇[8],與兒茶素反應(yīng)生成棕色素[9]等。此外,糠醛還可與葡萄酒中的硫化物反應(yīng),生成甲基呋喃硫醇,后者的閾值僅為0.4 ng/L,具有強(qiáng)烈的咖啡和烘烤氣味[10-11]。因此,在陳釀時(shí)間較短時(shí),糠醛和5-甲基糠醛的溶出量大于反應(yīng)量,其濃度上升;而隨著陳釀時(shí)間的延長(zhǎng),橡木中溶出的糠醛和5-甲基糠醛逐漸減少,而參與各種反應(yīng)的糠醛類化合物逐漸增多,因此,糠醛和5-甲基糠醛在葡萄酒中的含量逐漸減少。

圖1 陳釀過程中糠醛含量的變化Fig.1 Evolution of the concentration offurfural during wine aging

圖2 陳釀過程中5-甲基糠醛含量的變化Fig.2 Evolution of the concentration of5-methylfurfural during wine aging

2.2 陳釀過程中順式和反式橡木內(nèi)酯含量的變化

橡木內(nèi)酯可使葡萄酒產(chǎn)生橡木、堅(jiān)果氣味,尤其是順式橡木內(nèi)酯的含量,與葡萄酒中的橡木氣味具有顯著的正相關(guān)性(p<0.05)[12],而且不同品種的橡木,順反橡木內(nèi)酯的比值具有明顯差異,美國(guó)橡木及其陳釀的葡萄酒中,順反橡木內(nèi)酯的比值一般大于6,而法國(guó)橡木及其陳釀的葡萄酒中,順反橡木內(nèi)酯的比值僅為2左右[13-14]。從圖3和圖4可以看出,在90 d的陳釀過程中,葡萄酒中順反橡木內(nèi)酯的含量均隨陳釀時(shí)間延長(zhǎng)而顯著增加,且橡木片陳釀的葡萄酒,順反橡木內(nèi)酯的含量和比值均顯著低于橡木板陳釀的葡萄酒,尤其是在陳釀30 d以后,橡木片陳釀的葡萄酒中,順反橡木內(nèi)酯的溶出速率顯著低于橡木板陳釀的葡萄酒(p<0.05);從圖5可以看出,橡木片和橡木板陳釀的葡萄酒,順反橡木內(nèi)酯的比值均在6以上,且陳釀過程中,順反橡木內(nèi)酯之間的比例則隨陳釀時(shí)間延長(zhǎng)而逐漸下降。由于在葡萄酒微酸環(huán)境下,順反橡木內(nèi)酯之間極少發(fā)生相互轉(zhuǎn)化[15],因此陳釀過程中,順反橡木內(nèi)酯含量和比值的變化,一方面反映了在國(guó)產(chǎn)橡木中,順式橡木內(nèi)酯的含量明顯較反式橡木內(nèi)酯的含量多;另一方面則表明,在陳釀前期,順式橡木內(nèi)酯溶出速率相對(duì)較快,而在陳釀后期,反式橡木內(nèi)酯的溶出速率相對(duì)較快。Encarna[16]等在對(duì)采用法國(guó)和美國(guó)橡木桶進(jìn)行陳釀的研究中發(fā)現(xiàn),采用美國(guó)橡木桶陳釀的葡萄酒,順反橡木內(nèi)酯的比值隨陳釀時(shí)間延長(zhǎng)而逐漸下降,而采用法國(guó)橡木桶陳釀的葡萄酒,順反橡木內(nèi)酯含量之間的比值在陳釀過程中基本保持不變。

圖3 陳釀過程中順式橡木內(nèi)酯含量的變化Fig.3 Evolution of the concentration ofcis oak lactone during wine aging

圖4 陳釀過程中反式橡木內(nèi)酯含量的變化Fig.4 Evolution of the concentration oftrans oak lactone during wine aging

圖5 陳釀過程中順反橡木內(nèi)酯比值的變化Fig.5 Evolution of the ratio betweencis/trans oak lactone during wine aging

2.3 陳釀過程中香草醛含量的變化

香草醛是橡木中木質(zhì)素的熱解產(chǎn)物,可使葡萄酒產(chǎn)生宜人的香草氣味,對(duì)葡萄酒的陳釀香氣具有重要貢獻(xiàn)[17]。從圖6可以看出,在陳釀的前30 d,香草醛含量隨陳釀時(shí)間的延長(zhǎng)而顯著增加,且橡木片陳釀的葡萄酒中,香草醛含量顯著多于橡木板陳釀的葡萄酒;但在陳釀30 d以后,不同橡木制品陳釀的葡萄酒,香草醛含量表現(xiàn)出不同的變化趨勢(shì):橡木片陳釀的葡萄酒中,香草醛含量隨時(shí)間延長(zhǎng)而逐漸減少,而橡木板陳釀的葡萄酒中,香草醛含量則隨陳釀時(shí)間延長(zhǎng)而繼續(xù)增加,至60 d時(shí),橡木板陳釀的葡萄酒中香草醛含量已顯著高于橡木片陳釀的葡萄酒。這可能是由于雖然橡木片和橡木板中的香草醛含量具有差異,但葡萄酒對(duì)橡木片的浸漬速度要比橡木板的浸漬速率快,因此,在陳釀的前期,橡木板中香草醛的溶出速度較慢,而隨著陳釀時(shí)間的延長(zhǎng),橡木板內(nèi)部的香草醛逐漸溶出,而橡木片陳釀的葡萄酒,則由于香草醛溶出量的減少以及香草醛轉(zhuǎn)化為無芳香氣味的化合物[18]或與黃烷醇和花色苷發(fā)生加成反應(yīng)[19],使香草醛的含量出現(xiàn)下降趨勢(shì)。

圖6 陳釀過程中香草醛含量的變化Fig.6 Evolution of the concentrationof vanillin during wine aging

2.4 陳釀過程中愈創(chuàng)木酚和4-甲基愈創(chuàng)木酚含量的變化

愈創(chuàng)木酚和4-甲基愈創(chuàng)木酚也是橡木中木質(zhì)素的熱解產(chǎn)物,是使葡萄酒產(chǎn)生煙熏、烤肉氣味的主要物質(zhì)[20]。從圖7和圖8可以看出,在陳釀時(shí)間為20 d時(shí),葡萄酒中的愈創(chuàng)木酚和4-甲基愈創(chuàng)木酚含量即達(dá)到穩(wěn)定,此后其含量基本保持不變,而采用橡木片陳釀的葡萄酒,愈創(chuàng)木酚和甲基愈創(chuàng)木酚含量均顯著高于橡木板陳釀的葡萄酒,但在陳釀過程中,其含量均始終低于各自的閾值(75、65 μg/L)[21],這是由于愈創(chuàng)木酚和4-甲基愈創(chuàng)木酚兩種化合物主要是在橡木烘烤過程中產(chǎn)生的,且主要是在烘烤溫度達(dá)到230 ℃以上時(shí)才產(chǎn)生,而在200 ℃時(shí)生成的量較少[22],因此其在葡萄酒中的濃度較低。而由于橡木片和橡木板具有不同的傳熱系數(shù),在相同的烘烤條件下,橡木片和橡木板中愈創(chuàng)木酚類化合物的濃度也具有差異[23],這可能是采用橡木片和橡木板陳釀的葡萄酒中,愈創(chuàng)木酚含量產(chǎn)生差異的主要原因。

圖7 陳釀過程中愈創(chuàng)木酚含量的變化Fig.7 Evolution of the concentrationof guaiacol during wine aging

圖8 陳釀過程中4-甲基愈創(chuàng)木酚含量的變化Fig.8 Evolution of the concentration of4-methylguaiacol during wine aging

2.5 陳釀過程中4-乙基苯酚和乙基愈創(chuàng)木酚含量的變化

橡木中的木質(zhì)素在熱降解過程中可產(chǎn)生少量的4-乙基苯酚和乙基愈創(chuàng)木酚,這兩種化合物是使葡萄酒產(chǎn)生馬廄、藥水等不良?xì)馕兜闹饕衔颷24]。從圖9和圖10可以看出,在陳釀的前30 d,4-乙基苯酚和4-乙基愈創(chuàng)木酚的含量無顯著變化,僅在陳釀30 d或60 d以后,含量顯著增加,且4-乙基苯酚含量遠(yuǎn)高于乙基愈創(chuàng)木酚含量,但其濃度均低于其閾值(620、140 μg/L)[25],這是由于4-乙基苯酚和乙基愈創(chuàng)木酚,主要是由酒香酵母對(duì)酚酸脫羧還原產(chǎn)生的,它們的濃度主要取決于酒香酵母數(shù)量和底物的含量,而橡木對(duì)4-乙基苯酚和4-乙基愈創(chuàng)木酚的含量影響不大[26]。在陳釀前期,酒香酵母被二氧化硫抑制,產(chǎn)生的4-乙基苯酚和乙基愈創(chuàng)木酚較少;而隨著陳釀時(shí)間的延長(zhǎng),二氧化硫含量逐漸減少,酒香酵母活性增強(qiáng),因此,在陳釀后期,4-乙基苯酚和乙基愈創(chuàng)木酚的含量快速上升。Luis[8]等在對(duì)采用不同容積的橡木桶陳釀的葡萄酒進(jìn)行研究時(shí),也發(fā)現(xiàn)乙基苯酚和乙基愈創(chuàng)木酚的主要是在陳釀后期產(chǎn)生的,且橡木桶容積對(duì)乙基苯酚和乙基愈創(chuàng)木酚含量無顯著影響。

圖9 陳釀過程中4-乙基苯酚含量的變化Fig.9 Evolution of the concentration of4-ethylphenol during wine aging

圖10 陳釀過程中4-乙基愈創(chuàng)木酚含量的變化Fig.10 Evolution of the concentration of4-ethyl guaiacol during wine aging

3 結(jié)論

采用SPME-GC-MS檢測(cè)了采用國(guó)產(chǎn)橡木片和橡木板陳釀的葡萄酒主要陳釀香氣成分的變化。結(jié)果表明橡木片和橡木板陳釀的葡萄酒之間,除乙基苯酚和乙基愈創(chuàng)木酚無顯著差異外,糠醛、香草醛、愈創(chuàng)木酚和橡木內(nèi)酯的含量均具有顯著差異。上述幾種化合物的變化趨勢(shì)表明,一方面由于橡木片和橡木板具有不同的傳熱系數(shù),烘烤過程中產(chǎn)生的揮發(fā)性化合物含量將具有差異;另一方面,在陳釀過程中,葡萄酒對(duì)橡木片和橡木板中揮發(fā)性香氣成分的浸提速率也不同,因此,陳釀時(shí)間和橡木制品的類型將對(duì)葡萄酒中相關(guān)的陳釀香氣成分含量產(chǎn)生顯著的影響。

[1]Jarauta I,Cacho J,Ferreira V. Concurrent phenomena contributing to the formation of the aroma of wine during aging in oak wood:An analytical study[J]. Journal of Agricultural and Food Chemistry,2005,53(10):4166-4177.

[2]Arapitsas P,Antonopoulos A,Stefanou E,et al. Artificial aging of wines using oak chips[J]. Food Chemistry,2004,86(4):563-570.

[3]Hern NP,Franco E,Huerta CG,et al. Criteria to discriminate between wines aged in oak barrels and macerated with oak fragments[J]. Food Research International,2014,57(2):34-41.

[4]Simon BF,Sanz M,Cadahia E,et al. Chemical characterization of oak heartwood from Spanish forests of Quercus pyrenaica(Wild.). Ellagitannins,low molecular weight phenolic,and volatile compounds[J]. Journal of Agricultural and Food Chemistry,2006,54(21):8314-8321.

[5]Cadahia E,Simon B,Jalocha J. Volatile Compounds in Spanish,French,and American Oak Woods after Natural Seasoning and Toasting[J]. Journal of Agricultural and Food Chemistry,2003,51(20):5923-5932.

[6]Carrillo JD,Tena MT. Determination of volatile oak compounds in aged wines by multiple headspace solid-phase microextraction and gas chromatography-mass spectrometry(MHS-SPME-GC-MS)[J]. Analytical and bioanalytical chemistry,2006,385(5):937-943.

[7]Garde NT,Lorenzo C,Carto JM,et al. Effects of composition,storage time,geographic origin and oak type on the accumulation of some volatile oak compounds and ethylphenols in wines[J]. Food Chemistry,2010,122(4):1076-1082.

[8]Perezprieto LJ,Lopez JA,Martinez A,et al. Extraction and formation dynamic of oak-related volatile compounds from different volume barrels to wine and their behavior during bottle storage[J]. Journal of Agricultural and Food Chemistry,2003,51(18):5444-5449.

[9]Camara M,Gharbi N,Lenouvel A,et al. Detection and Quantification of Natural Contaminants of Wine by Gas Chromatography-Differential Ion Mobility Spectrometry(GC-DMS)[J]. Journal of Agricultural and Food Chemistry,2013,61(5):1036-1043.

[10]Tominaga T,Blanchard L,Darriet P,et al. A powerful aromatic volatile thiol,2-furanmethanethiol,exhibiting roast coffee aroma in wines made from several Vitis vinifera grape varieties[J]. Journal of Agricultural and Food Chemistry,2000,48(5):1799-1802.

[11]Gardecerd NT,Anca C. Review of quality factors on wine ageing in oak barrels[J]. Trends Food Sci Tech,2006,17(8):438-447.

[12]Bartista AB,Lencina AG,Cano LM,et al. The use of oak chips during the ageing of a red wine in stainless steel tanks or used barrels:effect of the contact time and size of the oak chips on aroma compounds[J]. Australian Journal of Grape and Wine Research,2008,14(2):63-70.

[13]Watehouse AL,Towey JP. Oak Lactone Isomer Ratio Distinguishes between Wine Fermented in American and French Oak Barrels[J]. Journal of Agricultural and Food Chemistry,1994,42(9):1971-1974.

[14]Mosedale JR,Puech JL,Feuillat F. The influence on wine flavor of the oak species and natural variation of heartwood components[J]. American Journal of Enology and Viticulture,1999,50(4):503-512.

[15]Pollnitz A. Analysis of volatile wine components derived from oak products during winemaking and storage[D]. Australia;University of Adelaide,2000.

[16]Gmezplaza E,Prezpireto LJ,Fernndez JI,et al. The effect of successive uses of oak barrels on the extraction of oak-related volatile compounds from wine[J]. International Journal of Food Science and Technology,2004,39(10):1069-1078.

[17]Underwood BJ. The effect of successive interpolations on retroactive and proactive inhibition[D]. Evanston,Ill.;University of Iowa,1945.

[18]Spillman PJ,Pollnitz AP,Liacopoulos D,et al. Formation and Degradation of Furfuryl Alcohol,5-Methylfurfuryl Alcohol,Vanillyl Alcohol,and Their Ethyl Ethers in Barrel-Aged Wines[J]. Journal of Agricultural and Food Chemistry,1998,46(2):657-663.

[19]BourdenMFN,Vivas N,Absalon C,et al. Structural diversity of nucleophilic adducts from flavanols and oak wood aldehydes[J]. Food Chemistry,2008,107(4):1494-1505.

[20]Brajkovich M,Tibbits N,Peron G,et al. Effect of Screwcap and Cork Closures on SO2 Levels and Aromas in a Sauvignon Blanc Wine[J]. Journal of Agricultural and Food Chemistry,2005,53(26):10006-100011.

[21]Pollnitz AP,Pardon KH,Sykes M,et al. The Effects of Sample Preparation and Gas Chromatograph Injection Techniques on the Accuracy of Measuring Guaiacol,4-Methylguaiacol and Other Volatile Oak Compounds in Oak Extracts by Stable[J].

Journal of Agricultural and Food Chemistry,2004,52(11):3244-3252.

[22]Campbell JI,Sykes M,Sefton MA,et al. The effects of size,temperature and air contact on the outcome of heating oak fragments[J]. Australian Journal of Grape and Wine Research,2005,11(3):348-354.

[23]Simon BF,Cadahia AE,Muino I,et al. Volatile Composition of Toasted Oak Chips and Staves and of Red Wine Aged with Them[J]. American Journal of Enology and Viticulture,2010,61(2):157-165.

[24]Suarez R,Suarez JA,Morata A,et al. The production of ethylphenols in wine by yeasts of the genera Brettanomyces and Dekkera:A review[J]. Food Chemistry,2007,102(1):10-21.

[25]Chatonnet P,Dubourdie D,Boidron JN,et al. The origin of ethylphenols in wines[J]. J Sci Food Agr,1992,60(2):165-178.

[26]Cerdan TG,Goni DT,Azpilicueta CA. Changes in the concentration of volatile oak compounds and esters in red wine stored for 18 months in re-used French oak barrels[J]. Australian Journal of Grape and Wine Research,2002,8(2):140-145.

Effect of different types of domestic oak products on wine aging aroma

LI Lan-xiao1,LI Ji-ming1,*,XU Yan1,2,FAN Wen-lai2,TANG Ke1,YU Ying1,HAN Peng1,ZHAO Rong-hua1

(1.Center of Science and Technology,Changyu Group Co. Ltd.,Yantai 264000,China;2.Laboratory of Brewing Microbiology and Applied Enzymology,Key Laboratory of Industrial Biotechnology,Ministry of Education,School of Biotechnology,Jiangnan University,Wuxi 214122,China)

The changes of the main aging aroma of wines that treated with oak chips and staves respectively made from Quercus mongolica were determined by solid-phase microextraction and gas chromatography-mass spectrometry during the aging process. The results showed that the concentrations of furfural and 5-methyl furfural were up to the maximum after 10 or 20 days,and then their contents decreased rapidly. The concentrations of guaiacol and methyl guaiacol reached their highest value after 20 days,and then remained constant. Trans and cis oak lactone content increased within 90 days during the aging process. The concentration of vanillin in wines treated with oak chips and staves changed in different trends:the concerntration of vanillin in wine that treated with oak chips reached the maximum after 30 days,and then decreased slowly,while the concerntration of vanillin in wine that treated with oak chips increased within 90 days during the aging process. The concerntration of ethyl guaiacol and ethyl phenol increased significantly after 30 and 60 days. There were significant differences between the concerntration of furfural,5-methyl furfural,vanillin,guaiacol and oak lactone,except for ethyl guaiacol and ethyl phenol,which showed that the style of oak products have an important influence on the main aging aroma of wines.

oak products;wine;aging aroma

2014-11-26

李蘭曉(1982-),男,碩士，工程師,研究方向:葡萄與葡萄酒，E-mail:lilanxiao123456@163.com。

*通訊作者:李記明(1966-),男,博士，研究員,研究方向:葡萄酒工藝和葡萄栽培，E-mail:zyljm@163.com。

山東省泰山學(xué)者計(jì)劃項(xiàng)目;煙臺(tái)市科技發(fā)展計(jì)劃項(xiàng)目(2013NC054)。

TS262.6

A

1002-0306(2015)15-0184-06

10.13386/j.issn1002-0306.2015.15.031