Optimization of the HS-SPME-GC/MS technique for the analysis of volatile compounds in caprine Coalho cheese using response surface methodology

BEZERRA, Taliana Kênia Alves; ARAÚJO, Ana Rita Ribeiro; ARCANJO, Narciza Maria de Oliveira; SILVA, Flávio Luís Honorato da; QUEIROGA, Rita de Cássia Ramos do Egypto; MADRUGA, Marta Suely

doi:10.1590/1678-457X.0035

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Research Paper • Food Sci. Technol (Campinas) 36 (1) • Jan-Mar 2016 • https://doi.org/10.1590/1678-457X.0035 copy

Optimization of the HS-SPME-GC/MS technique for the analysis of volatile compounds in caprine Coalho cheese using response surface methodology

Authorship SCIMAGO INSTITUTIONS RANKINGS

Abstract

Caprine Coalho cheese presents great potential for a typical protected designation of origin, considering that this traditional Brazilian cheese presents a slightly salty and acid flavor, combined with a unique texture. This study optimized the HS-SPME-GC-MS methodology for volatile analysis of Coalho cheese, which can be used as a tool to help in the identification of the distinctive aroma profile of this cheese. The conditions of equilibrium time, extraction temperature and time were optimized using the statistical tool factorial experimental design 2³, and applying the desirability function. After the evaluation, it was concluded that the optimum extraction conditions comprised equilibrium and extraction time of 20 and 40 minutes, respectively; and ideal extraction temperature of 45 °C. The optimum extraction of volatile compounds in goat Coalho cheese captured 32 volatile compounds: 5 alcohols, 5 esters, 3 ketones, 6 acids, 3 aldehydes, 3 terpenes, and 7 hydrocarbons.

Keywords:
dairy products; cheese; aromas; GC/MS

	Independent Variables			Response function
Assay	Equilibrium Time (minutes)*	Extraction Time (minutes)*	Extraction Temperature (°C)*	Number of Peaks
1	–(10)	–(20)	–(30)	16
2	+(30)	–(20)	–(30)	20
3	–(10)	+(60)	–(30)	24
4	+(30)	+(60)	–(30)	19
5	–(10)	–(20)	+(60)	23
6	+(30)	–(20)	+(60)	26
7	–(10)	+(60)	+(60)	30
8	+(30)	+(60)	+(60)	25
9	–α(3)	0(40)	0(45)	24
10	+α(37)	0(40)	0(45)	26
11	0(20)	–α(6)	0(45)	19
12	0(20)	+α(74)	0(45)	25
13	0(20)	0(40)	–α(20)	16
14	0(20)	0(40)	+α(70)	19
15	0(20)	0(40)	0(45)	29
16	0(20)	0(40)	0(45)	30
17	0(20)	0(40)	0(45)	28

Number	Compouds	C₁^a a Artisinal caprine cheese.	CV^b b % CV, percentage of coefficient of variation.	C₂^c c caprine cheese – 1.	CV	C₃^d d caprine cheese – 2.	CV	LRI^e e Linear retention indices.	ID^f f A, mass spectrum and LRI agree with those of an authentic compound ran on VF-5ms column. B, mass spectrum agrees with reference spectrum in the NIST/EPA/NIH mass spectral database and LRI agree with those in the literature (Adams, 2007; Madruga et al., 2013; Mottram, 2014).
Acohol
1	Ethanol	4.42	73	3.73	20	1.13	43	< 600	A
3	2-Butanol	ND^g g ND, not detected.	-	21.16	1	ND	-	< 600	A
8	3-methyl-1-Butanol	0.35	3	3.67	12	1.07	10	760	A/B
11	1-Pentanol	ND	-	0.16	104	0.55	87	< 600	A
26	2-methyl-1-Decanol	1.78	18	ND	-	ND	-	1160	A/B
Esters
4	Ethyl Acetate	0.87	63	1.77	99	2.01	70	< 600	A
12	Ethyl Butanoato	3.38	14	8.99	1	4.82	54	808	A/B
19	Ethyl Hexanoato	4.48	13	6.32	1	10.24	8	1007	A/B
28	Ethyl Octanoato	5.50	6	2.11	14	4.86	34	1198	A/B
30	Ethyl Decanoato	3.10	15	ND	-	ND	-	1404	A/B
Ketones
2	2-pentanone	3.64	18	3.4	18	1.70	53	< 600	A
7	3-hydroxy-2-Butanone	3.91	99	8.73	14	ND	-	722	A/B
15	2-Heptanone	2.32	7	4.2	12	1.53	11	899	A/B
Acids
5	Acetic acid	ND	-	0.89	5	15.20	3	< 600	A
13	Butanoic acid	2.96	10	4.02	32	3.10	20	823	A/B
14	Pentanoic acid	ND	-	3.09	6	0.73	23	880	A/B
20	Hexanoic acid	16.00	20	7.60	71	13.76	60	1016	A/B
27	Octanoic acid	1.47	50	0.02	2	4.17	34	1198	A/B
29	Decanoic acid	0.27	3	ND	-	ND	-	1401	A/B
Aldehydes
6	3-methylbutanal	0.61	54	0.95	38	0.26	7	< 600	A
17	Benzaldehyde	5.86	117	ND	-	ND	-	986	A/B
21	2-octenal	ND	-	ND	-	1.85	45	1033	A/B
Terpenes
16	α-Pinene	2.21	3	5.51	19	5.11	3	945	A/B
31	Copaene	0.83	141	1.32	14	2.56	65	1406	A/B
32	Caryophyllene	2.95	141	6.64	11	7.50	8	1460	A/B
Hydrocarbons
9	3-ethyl-2-methyl Pentane	0.29	73	0.12	39	0.91	67	765	A/B
10	Tolueno	0.18	21	0.66	33	0.59	30	789	A/B
18	Decane	14.14	8	1.38	10	5.60	1	1003	A/B
22	3-methyldecane	1.15	5	ND	-	1.78	7	1059	A/B
23	4-methyl-1-Decene	2.10	2	ND	-	ND	-	1069	A/B
24	Undecane	9.16	0	3.56	9	8.97	11	1104	A/B
25	4-methydecane	5.02	23	ND	-	ND	-	1118	A/B

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[1] *Corresponding author: msmadruga@uol.com.br