氣相色譜法內(nèi)標(biāo)法在測(cè)定白酒風(fēng)味物質(zhì)中的應(yīng)用一、材料與方法：1.1儀器裝置：氣相色譜儀配有FID撿測(cè)器電子天平(0.0001)，微量移液器1.2材料及試劑：色譜醇：無(wú)水乙醇、乙酸正戊酯、叔戊醇、2-乙基丁酸、乙醛、異丁醛、丙酮、甲酸乙酯、乙酸乙酯、乙縮醛、甲醇、異戊醛、2-戊酮、丁酸乙酯、仲丁醇、正丙醇、二乙氧基-2-甲基丁烷、二乙氧基異戊烷、異丁醇、乙酸異戊酯、戊酸乙酯、2-戊醇、正丁醇、活性戊醇、異戊醇、己酸乙酯、正戊醇、醋翁、庚酸乙酯、乳酸乙酯、正己醇、己酸丁酯、辛酸乙酯、三甲基毗嗪、四甲基毗嗪、乙酸、糠醛、苯甲醛、丙酸、2,3-丁二醇、異丁酸、1，2-丙二醇、丁酸、糠醇、異戊酸、戊酸、苯乙酸乙酯、乙酸苯乙酯、己酸、2-苯乙醇、庚酸、十四酸乙酯、辛酸、棕櫚酸乙酯、硬脂酸、油酸乙酯、亞油酸乙酯1.3色譜條件：毛細(xì)管柱色譜柱進(jìn)樣口溫度：200°C，檢測(cè)器溫度：230°C，載氣：氮?dú)?1ml/min)色譜柱升溫程序：35C保溫4min,4C/min升溫至60C,10C/min升到130C,15C/min升溫至205C保溫15min。1.4內(nèi)標(biāo)液的配制：取叔戊醇、乙酸正戊酯、2-乙基丁酸原液配成2%濃度的內(nèi)標(biāo)液。1.5白酒風(fēng)味成分混合標(biāo)液的配制：取風(fēng)味試劑按醇類、酯類、酸類、醛酮烷類按計(jì)劃添加量分別配制。在100ml容量瓶中，將每種風(fēng)味試劑按計(jì)劃添加量添加后，分別稱量其質(zhì)量，為實(shí)際添加質(zhì)量，并用色譜級(jí)乙醇定容，為標(biāo)樣原液。將標(biāo)樣原液用50%乙醇容液稀釋100倍后，按1%加入內(nèi)標(biāo)液，為標(biāo)樣使用液，其濃度為實(shí)際添加濃度。表1各風(fēng)味物質(zhì)標(biāo)樣含量配制表成分計(jì)劃添加濃度,mg/L計(jì)劃添加量,ml實(shí)際添加質(zhì)量，g實(shí)際添加濃度,mg/L1乙醛2002.001.5810158.102丙醛200.200.154215.423異丁醛100.100.07837.834丙酮100.100.07217.215甲酸乙酯1001.000.787278.726乙酸乙酯100010.009.0834908.347乙縮醛5005.004.1099410.998甲醇2002.001.5576155.769異戊醛1001.000.786278.62102-戊酮100.100.07857.8511丁酸乙酯2002.001.7923179.2312仲丁醇500.500.394839.4813正丙醇2002.001.6210162.1014異戊酸乙酯100.100.08458.4515異丁醇1001.000.783578.3516乙酸異戊酯300.300.08658.6517戊酸乙酯500.500.429042.90

182-戊醇500.500.371537.1519正」醇2002.001.6138161.3820活性戊醇500.500.411041.1021異戊醇5005.004.0344403.4422己酸乙酯100010.008.8122881.2223正戊醇500.500.389438.9424醋翁500.500.201320.1325庚酸乙酯200.200.175917.5926乳酸乙酯100010.0010.21771021.7727正己醇500.500.391439.1428己酸丁酯50.050.09449.4429三甲基毗嗪100.100.09479.4730辛酸乙酯500.500.442044.2031己酸異戊酯100.100.08588.5832乙酸100010.005.1960519.6033糠醛500.500.584458.4434四甲基毗嗪100.100.128712.8735壬酸乙酯100.100.08988.9836苯甲醛500.500.522252.2237丙酸500.500.487748.77382,3-丁二醇100.100.06846.8439異丁酸10.000.100.09149.1440癸酸乙酯10.000.100.08198.1941丁酸100.001.000.963196.3142糠醇10.000.100.05855.8543異戊酸10.000.100.09599.5944戊酸20.000.200.183618.3645苯乙酸乙酯10.000.100.104410.4446乙酸苯乙酯10.000.100.120612.0647己酸200.002.001.8034180.3448P-苯乙醇50.000.500.576457.6449庚酸10.000.100.09219.2150十四酸乙酯10.000.100.08348.3451辛酸10.000.100.08568.5652棕櫚酸乙酯10.000.100.08168.1653硬脂酸乙酯10.000.100.07507.5054油酸乙酯10.000.100.07827.8255亞油酸乙酯10.000.100.08088.081.6試驗(yàn)方法：1.6.1標(biāo)準(zhǔn)校正：取標(biāo)樣使用液混勻后進(jìn)樣川l進(jìn)行重復(fù)性校正。表2標(biāo)樣精密度和重復(fù)性試驗(yàn)成分標(biāo)樣1標(biāo)樣2標(biāo)樣3平均值RSD（%）1乙醛158.10163.18160.05160.441.602丙醛15.4215.1415.3015.290.913異丁醛7.837.817.857.830.274丙酮7.217.197.187.190.225甲酸乙酯78.7277.7978.3278.280.60

6乙酸乙酯908.34907.61908.03907.990.047乙縮醛410.99399.08405.89405.321.478甲醇155.76158.98157.69157.481.039異戊醛78.6278.1478.5178.420.32102-戊酮7.857.677.747.751.1611丁酸乙酯179.23177.56178.56178.450.4712仲丁醇39.4839.6739.5139.550.2613止丙醇162.10161.64161.98161.910.1514異戊酸乙酯8.458.378.458.420.5815異丁醇78.3579.5678.9978.970.7716乙酸異戊酯8.658.838.788.751.0517戊酸乙酯42.9042.5542.8142.750.43182-戊醇37.1537.3537.2537.250.2719止丁醇161.38160.48160.89160.920.2820活性戊醇41.1041.0041.2041.100.2421異戊醇403.44404.53404.12404.030.1422己酸乙酯881.22874.45879.15878.270.3923止戊醇38.9438.8838.8938.900.0824醋翁20.1320.3320.2220.230.4925庚酸乙酯17.5917.6217.6617.620.2026乳酸乙酯1021.771013.451018.291017.840.4127止己醇39.1440.6140.1239.961.8728己酸丁酯9.449.439.459.440.1129三甲基毗嗪9.479.189.409.351.6230辛酸乙酯44.2042.4643.1543.272.0331己酸異戊酯8.587.968.008.184.2632乙酸519.60487.09510.30505.663.3133糠醛58.4456.4057.0557.301.8234四甲基毗嗪12.8712.6412.7812.760.9235壬酸乙酯8.988.668.688.772.0536苯甲醛52.2250.7851.3651.451.4137丙酸48.7744.8046.5846.724.26382,3-丁二醇6.848.087.597.508.3339異丁酸9.148.128.998.756.2740癸酸乙酯8.197.247.847.766.2241丁酸96.3184.5789.4590.116.5542糠醇5.856.115.885.952.4343異戊酸9.599.179.129.292.7844戊酸18.3623.9220.1520.8113.6345苯乙酸乙酯10.4410.0510.2310.241.8946乙酸苯乙酯12.0611.8011.9811.951.1147己酸180.34171.10178.25176.562.74480-苯乙醇57.6455.4256.2456.431.9949庚酸9.2110.659.369.748.1150十四酸乙酯8.347.597.997.974.6951辛酸8.567.948.128.213.8852棕櫚酸乙酯8.167.418.137.905.3953硬脂酸乙酯7.507.207.417.372.11

54油酸乙酯7.828.127.897.941.9555亞油酸乙酯8.087.267.697.685.361.6.2樣品檢測(cè)：取10ul內(nèi)標(biāo)液+1.0ml樣品溶液，混勻后進(jìn)樣1Ml進(jìn)行檢測(cè)樣品中各風(fēng)味物質(zhì)的含量見表3：表3各風(fēng)味物質(zhì)含量表成分五糧液茅臺(tái)牛欄山精品52百年牛欄山1乙醛320.73964.526177.89124.572丙醛1.4310.3370.140.283異丁醛16.5150.7742.560.734丙酮66.8854.4082.772.225甲酸乙酯6.7851.4834.553.496乙酸乙酯421.12687.5391611.89451.317乙縮醛136.36121.897153.4077.068甲醇99.84781.25387.4453.569異戊醛34.00517.56102-戊酮50.7910.9211丁酸乙酯127.4814.95310.93131.5612仲丁醇39.33948.3488.5944.8213止丙醇137.1981089.285177.47175.0814異戊酸乙酯1.7020.4080.070.8515異丁醇82.99887.226119.9367.4116乙酸異戊酯1.6491.0293.342.1517戊酸乙酯61.3031.6161.5530.65182-戊醇173.7390.054.7819止丁醇30.44230.00813.2567.0420活性戊醇39.27859.28176.1941.1121異戊醇177.547194.884239.46151.8922己酸乙酯1235.5536.614.761410.4423止戊醇3.8365.0920.748.4324醋翁37.58286.57.3822.1025庚酸乙酯24.2481.0990.0214.8826乳酸乙酯539.325781.169703.40877.6227止己醇20.58911.7842.1233.1728己酸丁酯1.4080.3150.080.4029三甲基毗嗪0.0532.1570.230.9730辛酸乙酯12.3582.9881.674.4431己酸異戊酯2.360.2550.300.4232乙酸360.702877.829587.85453.6933糠醛34.848125.2952.6717.3834四甲基毗嗪0.3951.6770.4235壬酸乙酯0.1370.2620.3036苯甲醛0.6011.9710.170.6037丙酸23.12264.8156.0418.13382,3-丁二醇62.974354.649108.0339異丁酸4.3719.9921.568.82

40癸酸乙酯39.27859.2813.080.5241丁酸177.547194.8844.7488.1142糠醇1235.5536.65.752.4143異戊酸3.8365.0922.296.9944戊酸37.58286.524.4345苯乙酸乙酯39.27859.2810.6646乙酸苯乙酯177.547194.8840.680.1847己酸1235.5536.67.93631.85480-苯乙醇3.8365.0924.686.5449庚酸37.58286.51.0611.3650十四酸乙酯24.2481.0991.360.8651辛酸539.325781.1695.0352棕櫚酸乙酯3.370.6053硬脂酸乙酯0.0240.030.0354油酸乙酯0.0350.1143.270.1155亞油酸乙酯1.63標(biāo)樣色譜圖見圖1-1、圖1-2：^CT+tizawwroEocrr】頃ctmoonoo?-.urizmr-r<'TtrMr-.nijortMn'dm-ccpocmtrdomdojorniqft■：^ndciotkiikk：ilotiiiiiioiiiiiid^CT+tizawwroEocrr】頃ctmoonoo?-.urizmr-r<'TtrMr-.nijortMn'dm-ccpocmtrdomdojorniqft■：^ndciotkiikk：ilotiiiiiioiiiiiidr--卜卜卜-K+反cdbciodlllllll■lllllllllllllllllllllllll11IIIIIIIIII,_L,d_>D：i：i：i：iriEiZi11II1匚mg：r<i：go「此皿i*1i*i-T-mr-jciiSicciIIIIIIIIIIIIIIIIlliinr>gp「十汀40os■-■oidmzoofm苑泗匚fiycn?RccL「」TfEIDDCDijli：ir-i-+--r++-^hCi：i：i：ii：6cooIlliTT—T1rF■ITTTIIIILTIIIIIIIIIII IIIIIIIIIIII也寸ttn-Nd■頃OinT時(shí)>Dr--iT：it-CMCOiDh?coo而d守府—隹OJ回圖1-1標(biāo)樣色譜圖1IIIIIIIIlli11IIIIIIIIIIIIIIIIIIIIIIIIIIIIIIlliLi- ifliiODC4COO頃 l rrrh--iZi^lLir-fTOC> ii：■二n二fj flpi-fToamo groooorwog 頃 frotanio-s ic^ac■- 矛ggera >ziz； ddzioi■■'二 ■ 宣*蟲蟲疽甌扇 uW寸C-r-4 UT'J EOTOCXTTO5 CO OTTWOCTOCWOCO COCOOTTO uT-TTjij-IIIIIIIIIIIIIIIIIIIIIHillIIIIIIIlliIIIIIIIIlliI圖1-2標(biāo)樣色譜圖2樣品五糧液色譜圖見圖2-1、圖2-2：圖2-1樣品五糧液色譜圖1<>Ei'3-r-LCiLOn-f'TTr+HZri-r-O->?-FtiX!-「門5四!卜--4花>0■應(yīng)心寸心心曹>：>：>r<i：??