Scientia Agricultura Sinica ›› 2021, Vol. 54 ›› Issue (2): 379-391.doi: 10.3864/j.issn.0578-1752.2021.02.013

• FOOD SCIENCE AND ENGINEERING • Previous Articles     Next Articles

Dynamic Analysis for the Characteristics of Flavor Fingerprints for Brown Rice in Short-Term Storage Under High Temperature Stress

LIU Qiang(),LIU JiWei,TIAN Tian,YAN Wei,LIU Bing,ZHAO SiQi,HU QiuHui,DING Chao()   

  1. College of Food Science and Engineering, Nanjing University of Finance and Economics/Collaborative Innovation Center for Modern Grain Circulation and Safety/Jiangsu Key Laboratory of Quality Control and Further Processing of Cereals and Oil, Nanjing 210023
  • Received:2020-05-27 Accepted:2020-08-18 Online:2021-01-16 Published:2021-02-03
  • Contact: Chao DING E-mail:qiangliu@nufe.edu.cn;cding@nufe.edu.cn

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Abstract:

【Objective】 Changes of flavor fingerprinting in brown rice during high temperature short-term storage were investigated to establish a novel non-destructive detection methods for quality prediction of brown rice.【Method】 The brown rice with moisture content of 17.0 % (wet basis) was stored for 0, 5, 10, 15, 20 and 25 days under 40℃ temperature with relative humidity of 70%. Brown rice flavor compounds were collected by using headspace solid phase extraction method and its fingerprinting characteristics determined via gas chromatography-mass spectrometry (GC-MS) and gas chromatography-ion mobility spectrometry (GC-IMS). Dynamic principal component analysis (dPCA) model based on GC-IMS datasets was constructed.【Result】 Total of 42 volatile organic compounds were identified and quantitated based on GC-MS datasets. Aldehydes, alcohols and esters were the major compounds in flavor of fresh brown rice. After high temperature 15 days of storage, the contents of hexanal increased (P < 0.05) to (185.18±15.71) μg·kg-1 from initial contents of (81.09±0.53) μg·kg-1, and then sharply decreased to (12.89±0.72) μg·kg-1 aat 25 days of storage. Volatile organic compounds, including benzyl alcohol, 1-octene-3-ol and styrene, were successfully identified during storage stage. Based on GC-IMS analysis, ethyl acetate could be selected as the potential volatile markers to evaluate the freshness of brown rice. Good discriminated results were obtained for classifying different storage period of brown rice under via dPCA algorithm based on GC-IMS datasets. GC-IMS could better qualitatively analyze the volatile alcohols and ketones compounds than GC-MS. 【Conclusion】 GC-MS and GC-IMS detection method with dPCA discrimination analysis could obtain reliable flavor fingerprinting, achieve outstanding evaluation performance, and provide technical support for qualitative and quantitative monitoring the freshness of brown rice during high temperature storage.

Key words: brown rice, gas chromatography-mass spectrometry (GC-MS), gas phase ion migration spectrum (GC-IMS), volatile organic compounds, flavor fingerprint

Table 1

Varieties and contents of volatile organic compounds in brown rice during high temperature storage"

种类
Category		 名称
Name		 储藏时间 Storage time (d)
0 5 10 15 20 25
醛类 Aldehydes 正己醛 Hexanal 81.09±0.53b 71.28±1.84c 74.48±10.69bc 185.18±15.71a 59.67±9.07d 12.89±0.72e
苯甲醛 Benzaldehyde 136.92±28.06d 225.64±8.43b 176.47±5.96c 256.75±19.55a 126.52±17.77d 173.18±34.83cd
庚醛 Heptanal — 18.14±0.28 — — — —
反-2-辛烯醛 E-2-Octenal — 21.82±0.86a 22.91±1.85a — — —
反-2-十二烯醛 E-2-Dodecenal — — — — 15.34±2.13 —
醇类 Alcohols 己醇 Etnanol 115.10±20.88ab 109.93±3.36b 97.56±17.80ab 160.09±45.77a 121.80±19.14ab —
苯甲醇 Benzyl Alcohol — — 63.06±3.20b 109.33±2.84a 44.75±11.25c 124.43±45.33a
1-辛烯-3-醇 1-Octen-3-ol — 17.56±0.93c — — 125.97±20.45a 63.11±3.38b
正十三烷-1-醇 n-Tridecan-1-ol — 1.99±0.19 — — — —
酯类 Esters 丙位己内酯 4-Hexanolide 3.41±1.06 — — — — —
丙位壬内酯 γ-Nonanolactone — — 7.61±1.29 — — —
甲酸辛酯 Octyl Formate — — — — 17.58±0.78 —
酮类 Ketones 苯乙酮 Acetophenone — — — 4.01±2.29 — —
烃类 Hydrocarbons 十二烷 Dodecane 13.88±6.73c 19.22±1.22b 14.50±2.25c 24.09±7.28ab 24.43±1.50a 3.23±0.93d
葵环戊烷 Anemone 2.14±0.50b 5.42±0.19a — — — —
正十四烷 Tetradecane 7.90±1.25c 10.48±0.12b 14.75±3.56ab 9.38±2.95bc 18.25±0.91a 4.15±0.55d
长叶烯 d-Longifolene 13.16±3.92a 8.26±0.53b 15.87±0.11a 7.58±3.32b 14.29±2.89a 16.46±2.22a
环十四烷 Cyclotetradecane 6.43±1.98b 6.35±0.29b — 7.74±2.25b 12.04±2.71a —
8-己基十五烷 8-Hexylpentadecane 1.67±0.43b — — 2.87±0.79a — —
苯乙烯 Styrene — 14.83±0.28a 6.97±5.34b — — 3.21±0.10b
3,7-二甲基葵烷 3,7-Dimethyldecane — 5.62±0.22 — — — —
3,8-二甲基葵烷 3,8-Dimethyldecane — 11.67±1.1+ — — — —
壬基环丙烷 Nonylcyclopropane — 10.37±0.69a — — — 3.91±0.01b
二十烷 Eicosane — 4.19±1.70 — — — —
7-己基二十二烷 7-Hexyldocosane — 1.44±0.59 — — — —
1-十一烯 1-Undecene — — 7.25±0.69 — — —
十五烷 Pentadecane — — — 1.10±0.20 — —
十六烷 Hexadecane — — — 10.01±4.79 — —
十一烷 Undecane — — — 15.38±6.81 — —
1-戊烯 1-Pentene — — — 2.73±0.68 — —
9-甲基壬烷 9-Methylnonane — — — 14.41±1.95 — —
三十四烷 Tetradecane — — — — 3.70±1.94 —
其他 Others 氯乙酸十一酯 Undecyl Chloroacetate 6.12±5.12 — — — — —
邻二氯苯 1,2-Dichlorobenzene — 4.29±1.61 — — — —
1,3-二氯苯 1,3-Dichlorobenzene — — — 4.95±0.01 — —
三氟乙酸十六烷
Hexadecyl Trifluoroacetate		 — 4.87±1.10 — — — —
(甲氧基乙基)-基硫脲
4 - (Methoxyethyl) - Thiourea		 — — — — 1.19±0.05 —
酚类 Phenols 2,4-二叔丁基苯酚2,4-Di-Tert-Butylphenol 20.32±4.62e 40.07±2.57cd 36.42±4.30d 51.38±9.86c 212.01±12.56a 88.62±3.51b
2-叔丁基苯酚 o-Tert-Butyl Phenol — — 18.55±3.90 — — —
3-叔丁基苯酚 3-Tert-Butylphenol — — — 8.91±1.80b 22.98±0.91a —
4-叔丁基苯酚 4-Tert-Butylphenol — — 8.00±0.99 — — —
杂环 Heterocyclic 2,6-二叔丁基苯醌2,6-Di-Tert-Butyl-p-Benzoquinone 11.41±2.93c 11.36±0.86c 25.86±4.22b 38.80±6.99a 44.20±2.97a 21.00±2.43b

Fig. 1

Total contents of volatile organic compounds in brown rice Different letters on the bar chart in same type indicate significant differences (P<0.05)"

Fig. 2

Gas phase ion migration spectrogram of the samples Color scale from blue to red represents the signal intensity from -0.25 to 0.850; The different number represents the peak of identified compound based on GC-IMS database"

Fig. 3

Difference diagram of gas phase ion migration spectrogram of the sample a: Initial comparative signals in 0 d; b: The differential signals in 5th d; c: The differential signals in 10th d; d: The differential signals in 15th d; e: The differential signals in 20th d; f: the differential signals in 25th d"

Fig. 4

Aroma fingerprinting of volatile organic compounds selected from the GC-IMS The independent pixel represents the GC-IMS characteristic absorption peak. The color scale from blue to red represent the signal intensity from low to high, and black means the background"

Table 2

Compounds and relative contents corresponding to characteristic peaks of samples (%)"

序号Sequence 化合物
Compound		 储藏时间 Storage time (d)
0 5 10 15 20 25
1 乙醇Etnanol 8.79±0.30 9.15±0.24 9.12±0.08 9.51±0.28 12.09±0.21 13.19±0.14
2 3-甲基-3-丁烯-1-醇3-Methyl-3-buten-1-ol 2.21±0.09 2.39±0.05 2.62±0.09 2.77±0.16 3.54±0.06 4.49±0.21
3 2-甲基丁醇2-Methybutanol 1.17±0.05 1.27±0.03 1.45±0.04 1.53±0.03 1.92±0.05 2.39±0.06
4 戊醇1-Pentanol 2.80±0.15 2.89±0.10 2.80±0.08 1.80±0.07 1.42±0.06 1.26±0.10
5 3-甲基-1-戊醇3-Methyl-1-Pentanol 0.36±0.02 0.38±0.04 0.40±0.01 0.35±0.10 0.36±0.02 0.43±0.04
6 2-己醇2-Hexanol 2.77±0.07 3.09±0.10 3.19±0.12 3.50±0.10 4.66±0.02 5.15±0.11
7 叶醇Z-3-Hexen-1-ol 0.52±0.02 0.60±0.05 0.61±0.02 0.46±0.02 0.37±0.03 0.34±0.05
8 己醇1-Hexanol 0.44±0.04 0.42±0.05 0.44±0.01 0.43±0.03 0.44±0.05 0.48±0.05
9 甲基丙醇2-Methylpropanol 0.62±0.04 0.58±0.04 0.62±0.04 0.81±0.03 1.04±0.04 0.87±0.12
10 1-辛烯-3-醇1-Octen-3-ol 3.04±0.19 3.03±0.09 2.49±0.10 4.93±0.04 5.79±0.20 6.63±0.37
11 2-己基己醇2-Ethylhexanol 1.91±0.12 2.22±0.07 2.35±0.16 1.39±0.11 0.94±0.03 0.89±0.05
12 壬醇1-Nonanol 0.46±0.04 0.50±0.04 0.52±0.02 0.55±0.04 0.62±0.05 0.72±0.07
13 丁醇1-Butanol 0.60±0.03 0.64±0.02 0.70±0.03 1.02±0.06 0.92±0.05 1.02±0.07
14 2-甲基丙醇2-Methylpropanol 0.54±0.03 0.53±0.04 0.57±0.05 0.82±0.03 0.85±0.03 0.78±0.16
15 2-丁酮2-Butanone 2.87±0.06 3.07±0.08 3.03±0.08 1.99±0.11 2.05±0.03 2.31±0.24
16 2-戊酮2-Bentanone 2.80±0.04 3.01±0.04 2.97±0.18 2.84±0.08 3.09±0.04 2.86±0.29
17 2-己酮2-Bexanone 0.72±0.07 0.73±0.06 0.73±0.04 0.66±0.04 0.57±0.00 0.45±0.04
18 2-庚酮2-Beptanone 1.68±0.10 1.74±0.11 1.70±0.03 1.00±0.05 0.82±0.17 0.85±0.18
19 甲基己基甲酮2-Octanone 2.79±0.15 2.72±0.11 2.63±0.05 2.46±0.17 2.61±0.11 3.19±0.17
20 2-己酮2-Hexanone 0.25±0.03 0.32±0.04 0.28±0.02 0.34±0.04 0.47±0.03 0.62±0.10
21 丙酮Acetone 18.61±0.76 18.66±0.59 19.99±0.44 21.30±0.57 23.81±0.13 26.10±1.78
22 正己醛Hexanal 14.50±0.45 14.53±0.57 14.63±0.13 12.79±0.06 8.28±0.49 3.72±0.25
23 苯甲醛Benzaldehyde 7.91±0.21 7.90±0.25 7.66±0.29 9.19±0.02 10.51±0.21 8.95±0.58
24 辛醛Octanal 3.87±0.22 4.02±0.39 4.39±0.11 2.62±0.22 1.46±0.04 1.11±0.05
25 正壬醛n-Nonanal 5.23±3.37 3.25±0.41 3.02±0.07 3.49±0.08 3.51±0.36 3.69±0.43
26 戊醛Pentanal 0.88±0.07 0.79±0.14 0.80±0.06 0.48±0.04 0.21±0.04 0.14±0.01
27 反-2-辛烯醛E-2-Octenal 0.84±0.06 0.74±0.04 0.61±0.03 0.48±0.06 0.35±0.04 0.44±0.11
28 庚醛Heptanal 2.23±0.06 2.15±0.26 2.23±0.04 1.19±0.05 0.58±0.05 0.51±0.04
29 苯乙醛Phenylacetaldehyde 0.38±0.01 0.39±0.04 0.39±0.05 0.28±0.02 0.23±0.02 0.23±0.02
30 丁内酯Butyrolactone 0.13±0.03 0.15±0.01 0.12±0.01 0.11±0.02 0.14±0.03 0.13±0.02
31 乙酸丙酯Propyl acetate 0.49±0.08 0.36±0.06 0.27±0.03 0.20±0.02 0.20±0.01 0.14±0.03
32 2-戊基呋喃2-Pentylfuran 0.93±0.02 0.97±0.08 1.10±0.05 0.85±0.01 0.78±0.07 0.78±0.03
33 邻苯甲酚o-Cresol 6.49±0.29 6.62±0.54 5.32±0.19 7.66±0.18 5.26±0.39 5.02±0.55
34 对氯苯氧异丁酸p-Chlorophenoxyisobutyric acid 0.19±0.04 0.19±0.04 0.23±0.02 0.18±0.00 0.14±0.01 0.14±0.02

Fig. 5

Dynamic principal component analysis (dPCA) of the sample"

Table 3

Comparison of qualitative substance differences with two detection methods"

序号 Sequence 物质
Substance		 GC-MS GC-IMS
1 正己醛Hexanal + +
2 苯甲醛Benzaldehyde + +
3 庚醛Heptanal + +
4 反-2-辛烯醛E-2-Octenal + +
5 反-2-十二烯醛E-2-Dodecenal + -
6 辛醛Octanal - +
7 正壬醛n-Nonanal - +
8 戊醛Pentanal - +
9 苯乙醛Phenylacetaldehyde - +
10 乙醇Etnanol - +
11 3-甲基-3-丁烯-1-醇3-Methyl-3-buten-1-ol - +
12 2-甲基丁醇2-Methybutanol - +
13 戊醇1-Pentanol - +
14 3-甲基-1-戊醇3-Methyl-1-Pentanol - +
15 2-己醇2-Hexanol - +
16 叶醇Z-3-Hexen-1-ol - +
17 己醇1-Hexanol + +
18 甲基丙醇2-Methylpropanol - +
19 1-辛烯-3-醇1-Octen-3-ol + +
20 2-己基己醇2-Ethylhexanol - +
21 壬醇1-Nonanol - +
22 丁醇1-Butanol - +
23 2-甲基丙醇2-Methylpropanol - +
24 正十三烷-1-醇n-Tridecan-1-ol + -
25 2-甲基丙醇2-Methylpropanol - +
26 2-丁酮2-Butanone - +
27 2-戊酮2-Bentanone - +
28 2-己酮2-Bexanone - +
29 2-庚酮2-Beptanone - +
30 甲基己基甲酮2-Octanone - +
31 2-己酮2-Hexanone - +
32 丙酮Acetone - +
33 苯乙酮Acetophenone + -
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