สาขาอุตสาหกรรมเกษตร การประชุมทางวิชาการของมหาวิทยาลัยเกษตรศาสตร์ ครั้งที่ 57

Volatile Compounds in Robusta Instant Coffee

Yatip Puttatananun1 and Sasitorn Tongchitpakdee1*

ABSTRACT
The objective of this study was to determine volatile compounds profile of Robusta instant
coffee (agglomerated coffee powder) in comparison with volatile compounds profile of coffee powder
(spray dried coffee) and coffee extract. All samples were collected from commercial production
facility. Volatile compounds were extracted using headspace-solid phase microextraction (HS-SPME)
with DVB/CAR/PDMS fiber and were identified using gas chromatography-mass spectrometry (GC-
MS). The results showed profile of volatile compounds in coffee extract, coffee powder and instant
coffee were similar. These profiles consisted of volatile compounds including aldehyde, furans,
phenols, pyrazines, pyridines, and pyrroles. Among various volatile compounds, furans are the
predominant compounds in all samples, especially furfural (325.93 µg/g in coffee extract, 57.02 µg/g
in coffee powder and 35.29 µg/g in instant coffee solution). The results also showed that spray drying
resulted in loss of volatile compounds in coffee extract approximately 79-100%, while agglomeration
resulted in loss of volatile compounds in coffee powder approximately 28-52%.

Key Words: Robusta instant coffee, spray drying, volatile compounds profile
* Corresponding author; e-mail address: sasitorn.ch@ku.ac.th
1
Department of Food Science and Technology, Faculty of Agro-Industry, Kasetsart University, Bangkok 10900

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INTRODUCTION
Coffee has been the most commercialized food product and the most widely consumed
beverage in the world for decade (Clarke, 2001). Robusta coffee is one of the two cultivars which are
economically important in coffee market. It is easy to grow with higher yield when compared Arabica
coffee. Robusta coffee is widely grown in the Southern Part of Thailand and commercially used for
instant coffee production. The volatile compounds of coffee are largely due to for aroma. More than
950 compounds have been identified. Most of compounds increase during the roasting process. The
aroma profile of Arabica and Robusta coffee brews are different (Vitzthum et al., 1990). The roasty,
earthy and smoky /phenolic notes are more intense in the Robusta coffee. In coffee processing, green
bean is roasted to produce the characteristic flavor and associated with coffee beverage (Vincent,
1987). The coffee aroma during roasting is formed by pyrolysis, Strecker degradation, and Maillard
reaction (Vitzthum et al., 1990). The aroma of coffee is critical for consumer perception. Therefore,
during the several steps of instant coffee manufacturing process including extraction, evaporation,
spray drying and agglomeration, volatile compounds maybe lost. There is very little of information on
effect of processing on volatile compounds in Robusta instant coffee. The objective of this study was
to determine the flavor profile compounds in Robusta instant coffee (agglomerated coffee powder) in
comparison with volatile compounds profile of coffee powder (spray dried coffee) and coffee extract
in order to obtain information for improving product quality.

MATERIALS AND METHODS

1. Robusta instant coffee processing
Ground roasted coffee was extracted using hot water at 178 ◦C with pressure 12.7 bar in
extraction tank. Coffee extract samples were collected before spray drying, while coffee powder
samples were collected after spray drying at inlet temperature of 200◦C and outlet temperature of
117◦C. Instant coffee samples were collected after agglomeration process at 65◦C. All samples were
stored at -40 ◦C for further analysis.
2. Extraction volatile compounds by headspace-solid phase micro extraction (HS-SPME)
Coffee powder and instant coffee solutions were prepared using the manufacturer’s
instructions, by mixing 2 g of coffee with 120 mL of hot water. 25 µL of 5-Methyl-2-hexanone
(conc.83.0 mg/mL) was added to 5 g of each samples as internal standard. Then samples were
incubated for 15 minutes at 60 °C before exposed to headspace-solid phase micro extraction (HS-
SPME) with DVB/CAR/PDMS fiber for 30 minutes. SPME was injected into GC by direct thermal
desorption.

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สาขาอุตสาหกรรมเกษตร การประชุมทางวิชาการของมหาวิทยาลัยเกษตรศาสตร์ ครั้งที่ 57

3. Analysis the volatile compounds profile

The aroma volatile compounds analysis was performed in Gas Chromatography (model 6890,
Agilent) and using HP 5975 mass spectrometer. Compounds were separated on a capillary column
(CP-FFAP with 25m x 0.32 x 0.30 µm). Helium was used as carrier gas at a flow rate of 1.6 mL min-1.
Sample were injected with headspace-solid phase micro extraction (HS-SPME) in splitless mode.
The initial temperature column was as 50 °C hold for 2 minutes rising to 220 °C at a rate of 3 °C min -1
and hold for 20 minutes. The mass spectrometer operated in the electron ionization mode with an ion
source temperature 230 ◦C and a quad temperature of 150 °C. The mass range of m/z 40–400 amu
run in. The aroma volatile compounds were identified by comparing the mass spectra with those
known the compounds in the library with NIST library v.2.0g (2011) database and comparison with
retention index (RI) of standard alkane n-Alkane (C1-C28) with same column and condition (modified
from Akiyama et al., 2003).

RESULTS AND DISCUSSIONS

GC chromatograms showed that Robusta coffee extract, coffee powder (spray-dried) and
instant coffee (agglomerated) contained similar volatile compounds profiles (Fig 1). However, a
number of compounds were lost during instant coffee processing. The volatile compounds in each
sample were list in Table 1. The volatile compounds detected in the samples included aldehyde,
furans, phenols, pyrazines, pyridine and pyrroles. The results also showed that spray drying resulted
in loss of volatile compounds in coffee extract approximately 79 -100 %, while agglomeration resulted
in loss of volatile compounds in coffee powder approximately 28-52%.
IS

37
36
35

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IS
(b)

21
13

34
19

31,32
26

28
18

30
3
IS

(c)
13

21

34
19

31,32
26
18

28
3

30

Figure 1 Chromatogram of volatile compounds (a) coffee extracts (b) coffee powder (c) instant coffee
(1) Pyridine (2) 2-methoxymethylfuran (3) 2-methylpyrazine (4) 2,5-dimethylpyrazine (5) 2,6-
dimethylpyrazine (6) ethylpyrazine (7) 2-ethyl-6-methylpyrazine (8) 2-ethyl-5-methyl-yrazine (9) 2-
ethyl-3-methyl-pyrazine (10) 2,6-diethylpyrazine (11) 3-ethyl-2,5-dimethylpyrazine (12) 2-ethyl-3,5-
dimethylpyrazine (13) Furfural (14) 2-(methylsulfanylmethyl)furan (15) 3,5-diethyl-2-methylpyrazine
(16) 2acetylfuran (17) Benzaldehyde (18) 2-Furanmethanol, acetate (19) 5-ethyl-2-
Furancarboxaldehyde, (20) 2-acetyl-1-methyl pyrrole (21) 2-Furanmethanol (22) 2-furfuyl-5-methyl
furan (23) 2-Acetyl-3-methylpyrazine (24) Methyl salicylate (25) N-furfurylpyrrole (26) 2-
methoxyphenol (27) Maltol (28) 2-acetyl pyrrole (29) Difufurylether (30) Phenol (31)1H-Pyrrole-2-
carboxaldehyde (32) 4-ethyl-2-methoxyphenol (33) 1-methyl,1H-Pyrrole-2-carboxaldehyde (34) 2-
Methoxy-4-vinylphenol (35) Homosalate (36) Indole (37) 5-Hydroxymethylfurfural

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Table 1 Volatile compounds identified in coffee extracts, coffee powder and Instant coffee

Concentration(µg/g)
RIa Compounds Coffee Coffee Instant Odor Description b
extracts powder coffee
Aldehyde
1496 benzaldehyde 14.28 - 2.58 Sweet, cherry-almond,
anisic odor,
Furans
1478 2-acetylfuran 16.30 - - Sweet, almond, nutty, toast
ed, milky
1641 2-furanmethanol 143.12 29.99 14.99 Sulfuraceous, ester,
chemical
sweet, brown caramellike,
bready
1512 2-furanmethanol, acetate 28.17 4.79 2.27 Sweet fruity
1665 2-furfuyl-5-methyl-furan 5.74 - - -
1217 2-(methoxymethyl)-furan 2.37 - - Coffee roasted
1459 2-(methylsulfanylmethyl) 8.64 - - Onion, garlic, sulfurous,
furan pungent, vegetable
1533 5-methyl-2- 115.62 17.01 11.00 Sweet, caramellike, bread,
furancarboxaldehyde coffee
1450 Furfural 325.93 57.02 35.29 Sweet, brown, woody,
bready, with a slight
phenolic nuance,
caramellike
>1700 Difufurylether 28.72 - - Fruity, green, nut
>1700 5-hydroxymethylfurfural 83.56 - - Fatty, buttery, musty, waxy,
caramel-like
Phenol
>1700 Phenol 20.63 3.66 2.2 Spicy, burnt, smoky,
phenolic
>1700 2-methoxyphenol 42.36 8.01 5.01 Phenolic, smoky, spicy,
medicinal,
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>1700 2-methoxy-4-vinylphenol 255.78 19.48 14.02 Strong, spicy, dry, pungent,

smoky
>1700 4-ethyl-2-methoxy-phenol 75.55 5.33 2.53 Sweet, spicy, phenolic
medicinal
Pyrazines
1669 2-acetyl-3-methylpyrazine 20.12 - - Nutty, hazelnut, grain
1264 2,5-dimethylpyrazine 7.76 - - Chocolate, roasted nuts,
earthy
1319 2,6-dimethylpyrazine 6.13 - - Chocolate, roasted nuts,
1415 2,6-diethylpyrazine 3.09 - - Chocolate, roasted, nuts,
earthy
1240 2-methylpyrazine 26.25 8.12 6.9 Green, nutty, cocoa, musty
1380 2-ethyl-3-methyl-pyrazine 7.50 - -
1327 2-ethyl-6-methyl-pyrazine 11.95 - - Roasted potato
1375 2-ethyl-5-methyl-pyrazine 10.46 - - Green, earthy-musty, nutty,
cocoa
1434 2-ethyl-3,5-dimethylpyrazine 3.42 - - Cocoa, chocolate, nutty
1420 3-ethyl-2,5-dimethyl-pyrazine 12.91 - - Potato, cocoa, roasted,
nutty
1472 3,5-diethyl-2-methyl-pyrazine 7.05 - - Nutty, meaty
1324 ethylpyrazine 15.81 - - Nutty, musty, fermented,
coffee,
Pyridine
<1200 Pyridine 10.57 - - Grassy-green leaf, green
herbal
Pyrroles
>1700 1H-pyrrole2-carboxaldehyde 64.81 4.88 2.53 Musty, beefy, coffee
>1700 1-methyl,1H-Pyrrole-2- 37.41 - 2.68 Roasty, nutty
carboxaldehyde
>1700 2-acetylpyrrole 46.63 4.61 2.21 Musty, nutty-like with a
coumarin
>1700 2-acetyl 1-methlypyrrole 5.75 - - Nutty, floral, fruity, smoky,
musty

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>1700 N-furfurylpyrrole 18.49 - - Pungent,earthy,smoky

Others
>1700 Homosalate 22.26 - - Mild menthol
>1700 Indole 15.92 - - Floral
>1700 Maltol 39.61 - - Sweet, caramel, cotton
candy, burnt bready
>1700 Methyl salicylate 6.71 - - Sweet, root beer,
wintergreen phenolic,
camphoreous
a
Retention index calculated for the CP-FFAP capillary column
b
odor description from Flavor-base Pro 10th edition (2006)

Among various group of volatile compounds, furan groups are the most abundant volatile
compounds in highest in all samples. These results agreed with Budryn et al. (2011) who reported
that furans were the predominant volatile compounds in Robusta coffee. In general furans flavor
characteristic were known as sweet and caramellike. The furfural content is the most abundant
volatile compounds in coffee extract and coffee powder, although approximately 82.5% was
decreased during spray drying process. Chaichi et al., (2015) reported furfural concentrations were
decreased after coffee brewing with the boiling method and preparation of instant coffee.

Phenols also decreased approximately 92% after spray drying and agglomeration. Among
different phenols, 2-methoxy-4-vinylphenol was the most abundant in phenols group in all sample.
This compound presented with a smoky note. Puvipirom (2003) reported that 2-methoxy-4-
vinylphenol increased during roasting at 240 – 260 ◦C.

Other phenols detected included, 4-ethyl-2-methoxy-phenol and 2-methoxyphenol. 4-ethyl-2-

methoxy-phenol was predominant volatile compound in the Robusta coffee with spicy and earthy-
roasty perception (Blank et al., 1991). Similar to our results, Puvipirom (2003) also reported detection
of other volatile compounds in Robusta coffee such as 5-methy-2furancarboxaldehyde, 2-
furanmethanol, and 2-methoxyphenol, which gave greeny, nutty and roasted chili odor respectively.
The phenol groups are represented the smoky, astringent, spicy and phenolic like and also contribute
to the aroma of a cup of coffee (Clarke et al., 2001).

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CONCLUSION
Robusta coffee extract, coffee powder (spray-dried) and instant coffee (agglomerated)
contained similar volatile compounds profiles. However, significant loss of some volatile compounds
was observed during spray drying process, while agglomeration resulted in reduction of all volatile
compounds detected in coffee powder. Therefore, this instant coffee processing could be adjusted
maintain more volatile compounds.

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