SPME-gcMS提取分析口香糖香气成分
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从上面的TIC图看出来,固相微萃取SPME得到香气化合物比较丰富,峰数目较多。特别是后面的沸点高一些组分的提取效果也很好,响应高。总体灵敏度不错。
2.3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。由于FID的动态线性范围很宽,香气样品的含量范围较宽,一般用气相色谱FID来定量,而不用质谱总离子(TIC)来定量。用FID检测器的结果计算西瓜口香糖样品组分的含量。
Amdis拆分了9对共流峰,例如18.78, 19.08, 20.07, 31.40, 32.28(靠基线小峰),33.41(大峰里面小峰), 34.43(大峰里面小峰),42.01, 55.26min。
图2 Amdis拆分例子1
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图3 Amdis拆分例子2
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除去一些烷烃,萘类衍生物等基质带来的化合物外(已经删掉),这款口香糖共鉴定了112个组分。
含量参见下表。此西瓜味口香糖含清凉的薄荷酮,薄荷脑,WS23清凉剂,乙酸薄荷酯,柠稀,异松油烯,长叶烯及其它萜烯等薄荷油成分;含瓜香特征的西瓜醛,包括四个异构体和杂质;丰富的酯类香气物质,例如乙酸乙酯,丁酸乙酯,乙酸异戊酯,丁酸异戊酯,乙酸己酯,乙酸己烯酯异构体等。溶剂为三醋酸甘油酯,里面的二醋酸甘油酯,单醋酸甘油酯是其杂质。BHT为抗氧化剂。
2.4 口香糖成分
表 口香糖成分表
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No | RT | Name | Area% | ||
1 | 5.97 | ETHYL ACETATE | 0.403 | ||
2 | 7.46 | ETHYL PROPIONATE | 0.153 | ||
3 | 7.65 | ETHYL ISOBUTYRATE | 0.081 | ||
4 | 8.96 | ISOBUTYL ACETATE | 1.664 | ||
5 | 9.74 | ETHYL BUTYRATE | 7.625 | ||
6 | 10.19 | ETHYL METHYLBUTYRATE-2 | 0.048 | ||
7 | 10.52 | BIS-3-METHYLBUTYL ETHER | 0.003 | ||
8 | 10.92 | BUTYL ACETATE | 0.267 | ||
9 | 12.84 | ISOAMYL ACETATE | 7.061 | ||
10 | 14.43 | PHELLANDRENE ALPHA | 0.006 | ||
11 | 14.84 | AMYL ACETATE | 0.004 | ||
12 | 15.41 | METHYL CAPRONATE | 0.048 | ||
13 | 15.82 | LIMONENE | 0.290 | ||
14 | 16.07 | ISOAMYL ALCOHOL | 0.039 | ||
15 | 16.13 | EUCALYPTOL | 0.014 | ||
16 | 16.22 | PHELLANDRENE BETA | 0.009 | ||
17 | 16.71 | BUTYL BUTYRATE | 0.056 | ||
18 | 17.39 | ETHYL CAPRONATE | 0.820 | ||
19 | 18.78 | MENTHADIENE, 3,8-P- | 0.012 | ||
20 | 18.78 | ISOAMYL BUTYRATE | 1.582 | ||
21 | 19.08 | CYMENE, P- | 0.007 | ||
22 | 19.08 | HEXYL ACETATE | 1.209 | ||
23 | 19.27 | ISOAMYL METHYLBUTYRATE-2 | 0.007 | ||
24 | 19.49 | TERPINOLENE | 0.003 | ||
25 | 19.74 | MENTHADIENE, 2,4(8)-P- | 0.006 | ||
26 | 20.07 | ISOAMYL ISOVALERIANATE | 1.185 | ||
27 | 20.07 | BUTYL 3-METHYLBUTYRATE, 2-METHYL- | 1.136 | ||
28 | 20.64 | HEXENYL ACETATE, 3E- | 0.006 | ||
29 | 21.03 | HEXENYL ACETATE, 3Z- | 0.355 | ||
30 | 21.94 | METHYL HEPTENONE, 6,5,2- | 2.987 | ||
31 | 22.38 | ALCOHOL C 6 | 0.009 | ||
32 | 22.63 | MELONAL | 0.763 | ||
33 | 23.80 | HEXENOL, 3Z- | 0.294 | ||
34 | 24.56 | ETHLENE GLYCOL MONOBUTYL ETHER | 0.007 | ||
35 | 25.98 | ETHYL CAPRYLATE | 0.010 | ||
36 | 26.56 | Melonal isomer 1 | 0.092 | ||
37 | 26.94 | ACETIC ACID | 0.062 | ||
38 | 27.12 | Melonal Isomer 2 | 0.227 | ||
39 | 27.27 | MENTHONE | 0.144 | ||
40 | 27.76 | OCTYL ACETATE, 1- | 0.244 | ||
41 | 28.00 | SATIVENE, CYCLO- | 0.045 | ||
42 | 28.16 | MENTHOFURAN | 0.009 | ||
43 | 28.45 | ISOMENTHONE | 0.025 | ||
44 | 28.72 | LONGICYCLENE | 0.416 | ||
45 | 29.63 | Abitol I | 0.541 | ||
46 | 29.73 | LONGIFOLENE, ISO- | 0.051 | ||
47 | 29.91 | BENZALDEHYDE | 0.563 | ||
48 | 30.69 | Melonal isomer 3 | 0.404 | ||
49 | 31.03 | METHYL 3E-NONENOATE | 0.102 | ||
50 | 31.40 | MENTHYL ACETATE | 0.058 | ||
51 | 31.40 | ISOPULEGOL, NEO- | 0.063 | ||
52 | 31.70 | ISOPULEGOL | 5.353 | ||
53 | 32.09 | MENTHANYL FORMATE, 2-P-NEO | 0.244 | ||
54 | 32.28 | Melonal isomer 4 | 0.033 | ||
55 | 32.28 | NONADIENAL, 2E,6Z- | 0.009 | ||
56 | 33.14 | METHYL NONENOATE-2 | 14.300 | ||
57 | 33.14 | Caryophyleine-(I3) | 0.000 | ||
58 | 33.92 | NONANAL 1,2-PROPYLENE GLYCOL ACETAL P.1 | 0.085 | ||
59 | 34.04 | BUTYRIC ACID | 0.026 | ||
60 | 34.43 | MENTHOL | 15.228 | ||
61 | 34.43 | PANASINSENE, ALPHA- | 0.010 | ||
62 | 35.04 | 1,3-Propanediol, diacetate | 0.013 | ||
63 | 35.27 | DOWANOL DPnB | 0.020 | ||
64 | 35.43 | CURCUMENE, DIHYDRO-AR- | 0.023 | ||
65 | 36.53 | TERPINEOL, ALPHA- | 0.036 | ||
66 | 36.64 | BORNEOL | 0.007 | ||
67 | 37.07 | HIMACHALENE, BETA- | 0.025 | ||
68 | 37.29 | ACETYLFURAN-2 | 0.003 | ||
69 | 37.45 | ZINGIBERENE | 0.006 | ||
70 | 37.61 | MUUROLENE, ALPHA- | 0.023 | ||
71 | 37.91 | BENZYL ACETATE | 1.906 | ||
72 | 38.02 | CARVONE | 0.012 | ||
73 | 38.29 | DECANAL PROPYLENE GLYCOL ACETAL P.2 | 0.004 | ||
74 | 38.42 | STYRALLYL ISOBUTYRATE | 0.022 | ||
75 | 38.78 | GERANYL ACETATE | 0.059 | ||
76 | 39.28 | CADINENE, GAMMA- | 0.016 | ||
77 | 39.46 | CURCUMENE, ALPHA- | 0.016 | ||
78 | 39.66 | METHYL SALICYLATE | 0.004 | ||
79 | 40.29 | 1-Methoxy propane-2,3-diol Diacetate | 0.036 | ||
80 | 40.63 | ARBOROMA | 0.113 | ||
81 | 41.14 | DAMASCENONE, BETA- | 0.046 | ||
82 | 41.60 | CALAMENENE, CIS- | 0.030 | ||
83 | 42.01 | ETHYL LAURATE | 0.071 | ||
84 | 42.01 | COOLING AGENT WS23 | 5.784 | ||
85 | 42.01 | CAPRONIC ACID | 0.082 | ||
86 | 42.19 | IONONE, ALPHA- | 0.020 | ||
87 | 42.90 | HIMACHALENE, AR- | 0.014 | ||
88 | 43.13 | BENZYLALCOHOL | 1.368 | ||
89 | 44.40 | BHT | 1.325 | ||
90 | 44.58 | BORNYL SALICYLATE | 0.038 | ||
91 | 47.72 | ETHYLMALTOL | 0.801 | ||
92 | 48.34 | ETHYLGUAIACOL, 4- | 0.026 | ||
93 | 49.18 | CAPRYLIC ACID | 0.066 | ||
94 | 49.84 | TRIACETIN | 16.488 | ||
95 | 50.42 | MENTHOL, 8-HYDROXY, NEO- | 2.309 | ||
96 | 52.04 | DECALACTONE, GAMMA- | 0.053 | ||
97 | 52.22 | SCLAREOLOXIDE | 0.058 | ||
98 | 52.52 | PELARGONIC ACID | 0.081 | ||
99 | 52.67 | SCLAREOLOXIDE | 0.032 | ||
100 | 52.93 | MENTHOL, 8-HYDROXY- | 0.922 | ||
101 | 53.47 | MENTHANEDIOL, 2,8-P- P.1 | 0.089 | ||
102 | 54.38 | GLYCERIN DIACETATE (DIACETIN) | 0.032 | ||
103 | 55.13 | Abitol 4 | 0.025 | ||
104 | 55.26 | PHENOL, 2-TERT.-BUTYL-5-METHYL- | 0.027 | ||
105 | 55.26 | MONOACETIN | 0.007 | ||
106 | 55.46 | GAMMA UNDECALACTONE | 1.121 | ||
107 | 55.68 | CAPRIC ACID | 0.076 | ||
108 | 59.75 | DODECALACTONE, DELTA- | 0.012 | ||
109 | 59.99 | BENZOIC ACID | 0.025 | ||
110 | 60.67 | LAURIC ACID | 0.043 | ||
111 | 62.13 | VANILLIN | 0.043 | ||
112 | 64.06 | MYRISTIC ACID | 0.022 | ||
99.98 |