symmacros
第1楼2014/05/31
2 结果与讨论
2.1 实验结果
此粽子的香气很淡很弱,用一般的液液萃取、固相微萃取、同时蒸馏萃取等方法提取效果差,灵敏度低。用磁力吸附搅拌子提取粽子样品,简单方便,灵敏度高,有利于香气香味化合物的提取。但是要用到热脱附,设备较贵。
经过热脱附解析后,进入大体积冷阱进样口,进行GC进行分离。用一根毛细管通过分流器分流后分别进入MSD和FID。 这样一次同时得到总离子色谱图TIC和FID色谱图两个结果,方便定性和定量。即用GC-MS的TIC定性,GC-FID定量。同时得到TIC和FID的色谱图(见图1 TIC):
化合物标记后的简图:
2.2数据处理:
先用Amdis质谱数据解卷积处理质谱数据,减少本底干扰,对共流出峰拆分,提取出大峰下面的峰或隐藏在里面的色谱峰。同时用Amdis的MSL质谱数据库和工作站的PBM(L)质谱数据库检索,并结合保留指数来鉴定峰。所有保留指数均由标准样品测定。极少数没有保留指数的化合物,参照其它资料和以往的经验,在保证良好匹配度的情况下确认。用MS定性鉴定香气化合物,用GC-FID色谱图的内标法来计算含量(部分无校正因子的化合物采用1作为校正因子计算)。
2.3粽子的香气香味成分
表 粽子的香气香味表
NO | RT | Compound Name 香气香味化合物名称 | 含量[ppb] |
1 | 3.942 | BUTANON, 2- | 115 |
2 | 4.773 | ETHYLFURAN-2 | 191 |
3 | 5.213 | DIACETYL | 432 |
4 | 7.504 | BUTYLACETAT | 119 |
5 | 7.753 | ALDEHYD C 6 | 545 |
6 | 11.04 | HEPTANON-2 | 65 |
7 | 11.63 | LIMONEN | 92 |
8 | 12.08 | PYRAZIN | 1230 |
9 | 12.99 | PENTYLFURAN-2 | 135 |
10 | 13.45 | DODECEN, 1- | 203 |
11 | 13.9 | STYROL | 67 |
12 | 14.13 | METHYLPYRAZIN-2 | 1204 |
13 | 14.98 | ACETYLMETHYLCARBINOL | 4623 |
14 | 15.63 | PROPANOL, 2-OXO- | 278 |
15 | 16.58 | DIMETHYLPYRAZINE, 2,6- | 111 |
16 | 16.86 | ETHYLPYRAZINE, 2- | 79 |
17 | 17.14 | METHYLHEPTENON-6,5,2 | 90 |
18 | 17.3 | DIMETHYLPYRAZIN-2,3 | 122 |
19 | 17.77 | ALKOHOL C 6 | 165 |
20 | 19.43 | ALDEHYD C 9 | 107 |
21 | 20.27 | PYRAZINE, PROPYL- | 4 |
22 | 21.18 | DIMETHYLSTYROLPARA | 131 |
23 | 21.56 | PROPENE, 2-METHYL-1-PHENYL-1- | 149 |
24 | 22.14 | ACETIC ACID | 82 |
25 | 22.34 | FURFURAL | 482 |
26 | 23.37 | ETHYL-2-HEXANOL | 310 |
27 | 23.91 | ACETYLFURAN-2 | 58 |
28 | 24.51 | BENZALDEHYD | 568 |
29 | 25.56 | propionic acid | 28 |
30 | 26.68 | ISOBUYRIC acid | 24 |
31 | 28.55 | BUTYROLACTON GAMMA | 356 |
32 | 28.96 | BUTYRIC ACID | 24 |
33 | 29.02 | CYCLOHEXENON, 4-ISOPROPYL-2- | 121 |
34 | 29.36 | ACETOPHENON | 551 |
35 | 30.04 | FURFURYLALCOHOL | 520 |
36 | 31.25 | CAPROLACTON GAMMA | 154 |
37 | 32.05 | PROPIOPHENON | 17 |
38 | 32.38 | BENZYLACETAT | 2 |
39 | 32.81 | IONEN, DEHYDRO- | 153 |
40 | 32.98 | VALERIC ACID | 46 |
41 | 33.32 | Furanon, 2(5H)-, 5-ethyl- | 192 |
42 | 34.62 | DOWANOL DB | 446 |
43 | 35.11 | ACETOPHENON, 2-HYDROXY- | 104 |
44 | 35.86 | ACETOPHENONE, 3-ETHYL- | 114 |
45 | 36.74 | CAPRONIC ACID | 61 |
46 | 37.03 | GUAIACOL | 492 |
47 | 37.6 | BENZYLALCOHOL | 290 |
48 | 37.75 | ALCOHOL C11 | 228 |
49 | 38.72 | PHENYLETHYLALCOHOL | 327 |
50 | 39.19 | CHINOLIN | 140 |
51 | 40.22 | HEXANOIC ACID, 2-ETHYL- | 51 |
52 | 40.4 | HEPTANOIC ACID | 82 |
53 | 40.4 | MALTOL | 7230 |
54 | 40.73 | ALCOHOL C12 | 4452 |
55 | 42.02 | PHENOL | 996 |
56 | 42.41 | ALDEHYD C18 SOG. | 253 |
57 | 42.59 | PYRROLIDONE, 2- | 1435 |
58 | 42.72 | FURANONE, 4,4-DIMETHYL-3-HYDROXY-4,5-DH-2(3H)- | 179 |
59 | 43.06 | PROPANOL, 1-PHENOXY-2- | 938 |
60 | 43.76 | CAPRYLIC ACID | 33 |
61 | 43.9 | 2-Nonensaeure-y-lacton | 321 |
62 | 44.27 | PROPANOL, 2-PHENOXY-1- | 84 |
63 | 44.41 | CRESOL PARA | 66 |
64 | 45.6 | OCTENOIC ACID, 5Z- | 13 |
65 | 46.09 | PHENOXYETHYLALCOHOL | 6 |
66 | 46.22 | BOVOLID | 125 |
67 | 46.85 | EUGENOL | 9 |
68 | 47.04 | PELARGONIC ACID | 28 |
69 | 47.17 | TETRADECANOL | 1636 |
70 | 47.74 | VINYLGUAIACOL-4 | 2805 |
71 | 48.48 | METHYLHEXADECANOAT | 153 |
72 | 49.85 | DIMETHOXYPHENOL-2,6 | 76 |
73 | 49.85 | PYRANONE, 3,5-DIHYDROX- 6-METHYL2,3-DH-4- | 820 |
74 | 50.17 | CAPRIC ACID | 54 |
75 | 51.48 | DIHYDROACTINIDIOLIDE | 763 |
76 | 52.09 | ISOEUGENOL, TRANS- | 623 |
77 | 53.13 | HEXADECANOL | 3043 |
78 | 53.51 | PHENOL, 4-VINYL- | 19633 |
79 | 54.59 | CUMARIN | 85 |
80 | 54.7 | INDOL | 396 |
81 | 55.51 | SUCCINIMIDE | 644 |
82 | 55.93 | INDOL, 2-METHYL- | 71 |
83 | 56.06 | LAURIC ACID | 61 |
84 | 57.12 | DAMASCON, 3-HYDROXY-BETA- | 180 |
85 | 57.85 | VANILLIN | 952 |
86 | 58.66 | Alcohol C18 | 1063 |
87 | 59.74 | ACETOVANILLON | 48 |
88 | 62.08 | HYDROXYBOVOLIDE | 171 |
89 | 66.81 | PALMITIC ACID | 202 |
90 | 68.24 | HYDROXYBENZALDEHYD PARA | 840 |
Toltal (ppb) | 66765 |