气相色谱法内标法在测定白酒风味物质中的应用一、材料与方法：1.1仪器装置：气相色谱仪配有FID捡测器电子天平（0.0001），微量移液器1.2 材料及试剂：色谱醇：无水乙醇、乙酸正戊酯、叔戊醇、2-乙基丁酸、乙醛、异丁醛、丙酮、甲酸乙酯、乙酸乙酯、乙缩醛、甲醇、异戊醛、2-戊酮、丁酸乙酯、仲丁醇、正丙醇、二乙氧基-2-甲基丁烷、二乙氧基异戊烷、异丁醇、乙酸异戊酯、戊酸乙酯、2-戊醇、正丁醇、活性戊醇、异戊醇、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、三甲基吡嗪、四甲基吡嗪、乙酸、糠醛、苯甲醛、丙酸、2，3-丁二醇、异丁酸、1，2-丙二醇、丁酸、糠醇、异戊酸、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、棕榈酸乙酯、硬脂酸、油酸乙酯、亚油酸乙酯1.3 色谱条件：毛细管柱色谱柱进样口温度：200℃，检测器温度：230℃，载气：氮气（1 ml /min）色谱柱升温程序：35℃保温4 min，4℃/ min升温至60℃，10℃/ min升到130℃，15℃/ min升温至205℃保温15 min。
1.4 内标液的配制：取叔戊醇、乙酸正戊酯、2-乙基丁酸原液配成2%浓度的内标液。
1.5 白酒风味成分混合标液的配制：取风味试剂按醇类、酯类、酸类、醛酮烷类按计划添加量分别配制。
在100ml容量瓶中，将每种风味试剂按计划添加量添加后，分别称量其质量，为实际添加质量，并用色谱级乙醇定容，为标样原液。
将标样原液用50%乙醇容液稀释100倍后，按1%加入内标液，为标样使用液，其浓度为实际添加浓度。
表1 各风味物质标样含量配制表成分计划添加浓度,mg/L计划添加量,ml实际添加质量，g实际添加浓度,mg/L 1乙醛200 2.00 1.5810158.102丙醛200.200.154215.423异丁醛100.100.07837.834丙酮100.100.07217.215甲酸乙酯100 1.000.787278.726乙酸乙酯100010.009.0834908.347乙缩醛500 5.00 4.1099410.998甲醇200 2.00 1.5576155.769异戊醛100 1.000.786278.62102-戊酮100.100.07857.8511丁酸乙酯200 2.00 1.7923179.2312仲丁醇500.500.394839.4813正丙醇200 2.00 1.6210162.1014异戊酸乙酯100.100.08458.4515异丁醇100 1.000.783578.3516乙酸异戊酯300.300.08658.6517戊酸乙酯500.500.429042.90182-戊醇500.500.371537.1519正丁醇200 2.00 1.6138161.3820活性戊醇500.500.411041.1021异戊醇500 5.00 4.0344403.4422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50.050.09449.4429三甲基吡嗪100.100.09479.4730辛酸乙酯500.500.442044.2031己酸异戊酯100.100.08588.5832乙酸100010.00 5.1960519.6033糠醛500.500.584458.4434四甲基吡嗪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100.100.0684 6.8439异丁酸10.000.100.09149.1440癸酸乙酯10.000.100.08198.1941丁酸100.00 1.000.963196.3142糠醇10.000.100.0585 5.8543异戊酸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200.00 2.00 1.8034180.3448β-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棕榈酸乙酯10.000.100.08168.1653硬脂酸乙酯10.000.100.07507.5054油酸乙酯10.000.100.07827.8255亚油酸乙酯10.000.100.08088.081.6 试验方法：1.6.1 标准校正：取标样使用液混匀后进样1μl进行重复性校正。
表2 标样精密度和重复性试验成分标样1标样2 标样3 平均值RSD(%) 1乙醛158.10163.18160.05160.44 1.60 2丙醛15.4215.1415.3015.290.91 3异丁醛7.837.817.857.830.27 4丙酮7.217.197.187.190.22 5甲酸乙酯78.7277.7978.3278.280.607乙缩醛410.99399.08405.89405.32 1.47 8甲醇155.76158.98157.69157.48 1.03 9异戊醛78.6278.1478.5178.420.32 102-戊酮7.857.677.747.75 1.16 11丁酸乙酯179.23177.56178.56178.450.47 12仲丁醇39.4839.6739.5139.550.26 13正丙醇162.10161.64161.98161.910.15 14异戊酸乙酯8.458.378.458.420.58 15异丁醇78.3579.5678.9978.970.77 16乙酸异戊酯8.658.838.788.75 1.05 17戊酸乙酯42.9042.5542.8142.750.43 182-戊醇37.1537.3537.2537.250.27 19正丁醇161.38160.48160.89160.920.28 20活性戊醇41.1041.0041.2041.100.24 21异戊醇403.44404.53404.12404.030.14 22己酸乙酯881.22874.45879.15878.270.39 23正戊醇38.9438.8838.8938.900.08 24醋翁20.1320.3320.2220.230.49 25庚酸乙酯17.5917.6217.6617.620.20 26乳酸乙酯1021.771013.451018.291017.840.41 27正己醇39.1440.6140.1239.96 1.87 28己酸丁酯9.449.439.459.440.11 29三甲基吡嗪9.479.189.409.35 1.62 30辛酸乙酯44.2042.4643.1543.27 2.03 31己酸异戊酯8.587.968.008.18 4.26 32乙酸519.60487.09510.30505.66 3.31 33糠醛58.4456.4057.0557.30 1.82 34四甲基吡嗪12.8712.6412.7812.760.92 35壬酸乙酯8.988.668.688.77 2.05 36苯甲醛52.2250.7851.3651.45 1.41 37丙酸48.7744.8046.5846.72 4.26 382，3-丁二醇 6.848.087.597.508.33 39异丁酸9.148.128.998.75 6.27 40癸酸乙酯8.197.247.847.76 6.22 41丁酸96.3184.5789.4590.11 6.55 42糠醇 5.85 6.11 5.88 5.95 2.43 43异戊酸9.599.179.129.29 2.78 44戊酸18.3623.9220.1520.8113.63 45苯乙酸乙酯10.4410.0510.2310.24 1.89 46乙酸苯乙酯12.0611.8011.9811.95 1.11 47己酸180.34171.10178.25176.56 2.74 48β-苯乙醇57.6455.4256.2456.43 1.99 49庚酸9.2110.659.369.748.11 50十四酸乙酯8.347.597.997.97 4.69 51辛酸8.567.948.128.21 3.88 52棕榈酸乙酯8.167.418.137.90 5.39硬脂酸乙酯55亚油酸乙酯8.087.267.697.68 5.361.6.2 样品检测：取10ul内标液+1.0ml 样品溶液，混匀后进样1μl进行检测样品中各风味物质的含量见表3：表3 各风味物质含量表成分五粮液茅台牛栏山精品52百年牛栏山1乙醛320.73964.526177.89 124.57 2丙醛 1.4310.3370.14 0.28 3异丁醛16.5150.774 2.56 0.73 4丙酮66.885 4.408 2.77 2.22 5甲酸乙酯 6.785 1.483 4.55 3.49 6乙酸乙酯421.12687.5391611.89 451.31 7乙缩醛136.36121.897153.40 77.06 8甲醇99.84781.25387.44 53.56 9异戊醛34.00517.56 102-戊酮50.7910.9211丁酸乙酯127.481 4.95310.93 131.56 12仲丁醇39.33948.3488.59 44.82 13正丙醇137.1981089.285177.47 175.08 14异戊酸乙酯 1.7020.4080.07 0.85 15异丁醇82.99887.226119.93 67.41 16乙酸异戊酯 1.649 1.029 3.34 2.15 17戊酸乙酯61.303 1.616 1.55 30.65 182-戊醇17 3.7390.05 4.78 19正丁醇30.44230.00813.25 67.04 20活性戊醇39.27859.28176.19 41.11 21异戊醇177.547194.884239.46 151.89 22己酸乙酯1235.553 6.614.76 1410.44 23正戊醇 3.836 5.0920.74 8.43 24醋翁37.58286.57.38 22.10 25庚酸乙酯24.248 1.0990.02 14.88 26乳酸乙酯539.325781.169703.40 877.62 27正己醇20.58911.784 2.12 33.17 28己酸丁酯 1.4080.3150.08 0.40 29三甲基吡嗪0.053 2.1570.23 0.97 30辛酸乙酯12.358 2.988 1.67 4.44 31己酸异戊酯 2.360.2550.30 0.42 32乙酸360.702877.829587.85 453.69 33糠醛34.848125.295 2.67 17.38 34四甲基吡嗪0.395 1.6770.42 35壬酸乙酯0.1370.2620.30 36苯甲醛0.601 1.9710.17 0.60 37丙酸23.12264.815 6.04 18.13 382，3-丁二醇62.974354.649108.03 39异丁酸 4.3719.992 1.56 8.8240癸酸乙酯39.27859.281 3.08 0.52 41丁酸177.547194.884 4.74 88.11 42糠醇1235.553 6.6 5.75 2.41 43异戊酸 3.836 5.092 2.29 6.99 44戊酸37.58286.524.43 45苯乙酸乙酯39.27859.2810.66 46乙酸苯乙酯177.547194.8840.68 0.18 47己酸1235.553 6.67.93 631.85 48β-苯乙醇 3.836 5.092 4.68 6.54 49庚酸37.58286.5 1.06 11.36 50十四酸乙酯24.248 1.099 1.36 0.86 51辛酸539.325781.169 5.03 52棕榈酸乙酯 3.37 0.60 53硬脂酸乙酯0.0240.030.03 54油酸乙酯0.0350.114 3.27 0.11 55亚油酸乙酯 1.63标样色谱图见图1-1、图1-2：图1-1 标样色谱图1图1-2 标样色谱图2样品五粮液色谱图见图2-1、图2-2：图2-1 样品五粮液色谱图1图2-2 样品五粮液色谱图2。