Hisorb probe萃取使用热脱附分析利趣拿铁香气成分

zwq1973

2017/09/05

私聊

气质联用（GCMS）

前言
利趣拿铁是一种咖啡饮料，其配料成分有：水、白砂糖、全脂奶粉、脱脂奶粉、咖啡粉、食品添加剂（碳酸氢钠、蔗糖脂肪酸酯、安赛蜜）、食用香料。一般对饮料的挥发性香气成分分析常见前处理方式主要有：spme，液液萃取，同时蒸馏萃取，热脱附等。现MARKES有一款Hisorb probe推出并结合热脱附进样，还未见大量使用，本文使用Hisorb probe萃取结合热脱附进行利趣拿铁挥发性香气成分分析研究。
1 实验部分
1.1 仪器和装置
美国安捷伦6890N/5973N气质联用仪
英国markes TD-100热脱附
英国markes Hisorb-P1萃取探针（pdms涂层）

1.2 样品
三得利利趣拿铁（超市购买）
1.3 gc/MS、热脱附条件
1.3.1气相条件
HP-INNOWAX（60m×0.32mm×0.25um）；载气：氦气；流量：1.0ml/min；程序升温：起始温度57℃(保留2min)，以4℃/min升到260℃（保留20min）；
1.3.2 质谱条件
EI源，70ev；辅助线温度：280℃；全扫描模式，质量扫描范围：29-420amu；四极杆150℃；离子源230℃。使用自建库，nist14库，wiley库并结合已有的保留指数进行定性，tic面积百分比进行定量
1.3.3热脱附条件
Prepurge time 5min，tube desorb time5min，tube desorb Temp 280℃，trap low Temp -20℃，trap heatingrate MAX℃/s，trap high Temp 280℃。
1.4 样品前处理
取10ml样品于20ml顶空瓶，将探针浸入液面，常温下磁力搅拌萃取30min。
2结果和讨论
样品的总离子流图如下

总共检出107个物质，具体见下表

Name	RT	百分含量
acetone	5.4776	0.334
2-methylfuran	5.9055	0.164
butanal	5.9747	0.009
2-butanone	6.2284	0.151
2-methyl butanal	6.3963	0.734
isovaleral	6.4423	0.181
ethanol	6.5247	0.070
benzene	6.7934	0.104
ethyl propionate	6.935	0.259
2-pentanone	7.3024	0.132
ethyl butanoate	8.3222	0.272
3-hexanone	8.7306	0.032
dimenthyl disulphide	9.3225	0.072
hexanal	9.4409	0.059
isovaleral PG acetal	11.5817	0.232
2-heptanone	12.1034	2.659
pyridine	12.1148	1.895
methyl hexanoate	12.184	0.051
2,4,5-trimethyloxazole	12.3616	0.032
Methyl thiobutanoate	12.6247	0.173
2-methyl pyridine	13.0991	0.033
furfuryl methyl ether	13.7457	0.036
4,5-diethyl oxazole	13.992	0.021
2-methyl pyrzaine	14.6749	0.285
octanal	15.3993	0.033
3-methyl pyridine	15.5623	0.034
acetol	15.7977	0.154
2-heptanone PG ketal	15.9861	0.251
2,5-dimethyl pyrzaine	16.4564	0.126
2,6-dimethyl pyrazine	16.6336	0.161
2-ethyl pyrazine	16.8466	0.201
2,3-dimethyl pyrazine	17.25	0.008
2-methoxy-3-methyl pyrzaine	18.0832	0.098
3-ethyl pyridine	18.3701	0.249
2-ethyl-5(or6)-methyl pyrazine	18.4693	0.236
2-nonanone	18.5731	2.837
2-ethyl-5(or6)-methyl pyrazine	18.69	0.156
nonanal	18.7448	0.096
2,3,5-trimethyl pyrzaine	19.0721	0.093
2-methyl-3-ethyl pyrzaine	19.0844	0.069
2-propyl pyrazine	19.54	0.011
ethyl octanoate	19.965	0.007
2,6-diethyl pyrzaine	20.0337	0.086
2-ethyl-3，6-dimethyl pyrzaine	20.3296	0.265
acetic acid	20.5022	0.537
2,3-dimethy-5-ethyl pyrzaine	20.8628	0.096
furfuryl	21.0194	0.472
2-ethyl-1-hexanol	21.5489	0.197
2,3-Diethyl-5-Methyl pyrazine	21.836	0.006
furfuryl methyl sulfide	21.7729	0.067
2,6-Diethyl-3-methylpyrazine	21.8913	0.073
pentadecane	21.9159	0.054
decanal (aldehyde C-10)	22.0816	0.136
2-Nonanone PG Ketal	22.2919	0.154
formic acid	22.5947	0.060
benzaldehyde	23.0227	0.246
propanoic acid	24.353	0.007
Octanol	23.6519	0.505
5-methyl furfural	24.455	0.157
1,2-propylene glycol	24.649	0.551
methyl decanoate	24.9645	0.109
2-undecanone	25.1143	1.427
4-Terpineol	25.2586	0.013
2-furfuryl furan	25.4516	0.018
2-methyl-3-butyl pyrazine	25.8382	0.023
ethyl decanoate	26.2288	0.105
furfuryl acetone	26.5293	0.016
furfuryl alcohol	26.8002	0.330
butyl butyryl lactate	29.2438	0.852
decanol	29.6399	0.012
2-hydroxy-2-Cyclopenten-1-one	30.0369	0.083
2-tridecanone	31.1478	0.468
Corylone=MCP	31.6545	0.033
1-furfuryl pyrrole	31.7652	0.087
hexanoic acid	32.002	0.088
guaiacol	32.5569	0.205
benzyl alcohol	32.9339	1.023
maltol	34.6549	0.020
2-acetyl pyrrole	35.4576	0.037
difurfuryl ether	35.7758	0.091
Ethyl maltol	36.5589	0.486
2-formyl pyrrole	36.851	0.017
4-ethyl guaiacol	36.9386	0.328
gamma-nonalactone (aldehyde C-18 (so-called))	37.1162	10.467
Ethyl tetradecanoate	37.3138	0.051
octanoic acid	37.493	0.015
methyl 4-tert-butyl phenyl acetate	37.7181	0.693
triacetin	37.8624	0.405
sulfuryl acetate	39.4409	0.079
4-vinyl guaiacol	40.9174	0.215
delta-decalactone	41.0818	0.785
2-formyl-N-furfuryl-pyrrole	42.2738	0.065
decanoic acid	42.4399	1.198
gamma-undecalactone (aldehyde C-14 (so-called))	42.5647	17.734
2,4-di-tert.-butyl-phenol	43.3086	0.059
delta-undecalactone	43.7029	1.471
gamma-dodecalactone	45.0797	0.205
delta-dodecalactone	46.2384	28.997
Dodecanoic acid	46.9969	1.345
Vanillin	48.9319	5.701
12-methyl tridecanoic acid	50.2186	0.132
Tetradecanoic acid	51.2066	3.023
12-methyl Tetradecanoic acid	52.5861	0.026
Pentadecanoic acid	53.2107	0.142
14-methyl Pentadecanoic acid	54.2866	0.015
n-Hexadecanoic acid	55.3725	3.340
Caffeine	62.5146	1.487

分析结果中含有大量的吡嗪，吡啶，吡咯，噻唑，呋喃，愈创木酚等类些化合物是咖啡香气重要的组成部分。同时2-位酮，脂肪酸类，内酯类化合物有恰恰是奶味香气特征化合物。
Hisorb萃取探针在使用上感觉就是大号的spme萃取头，不过涂层相对比较厚，且需要使用热脱附来进行进样，类似于搅拌吸附转子。至于它和spme，搅拌转子在分析效果上的差异，有待下次研究。