Subcritical Extraction of <i>Salvia hispanica</i> L. Oil with <i>N</i>-Propane: Composition, Purity and Oxidation Stability as Compared to the Oils Obtained by Conventional Solvent Extraction Methods

Zanqui, Ana B.; Morais, Damila R. de; Silva, Cláudia M. da; Santos, Jandyson M.; Chiavelli, Lucas U. R.; Bittencourt, Paulo R. S.; Eberlin, Marcos N.; Visentainer, Jesui V.; Cardozo-Filho, Lúcio; Matsushita, Makoto

doi:10.5935/0103-5053.20140278

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Journal of the Brazilian Chemical Society

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Articles • J. Braz. Chem. Soc. 26 (2) • Feb 2015 • https://doi.org/10.5935/0103-5053.20140278 copy

Subcritical Extraction of Salvia hispanica L. Oil with N-Propane: Composition, Purity and Oxidation Stability as Compared to the Oils Obtained by Conventional Solvent Extraction Methods

Authorship SCIMAGO INSTITUTIONS RANKINGS

This study evaluated the Chia (Salvia hispanica L.) oil composition in terms of fatty acids (FA), sterols, acylglycerols and oxidative stability obtained via subcritical n-propane fluid extraction (SubFE-propane), in different temperatures and pressure conditions, as compared to Bligh & Dyer (BD), Soxhlet (SE) and Folch (FLS) extractions. Total lipid varied from 23.25 to 30.21% and the best yield was obtained by both SubFE-propane extraction at 45 ºC and 12 MPa (A). α-Linolenic acid (18:3n-3) was the most abundant FA and SubFE-propane extraction provided the best results for the sum of n-3 and PUFA. All oil samples were similar in regard to triacylglycerols (TAG) profiles as measured via direct electrospray ionization mass spectrometry (ESI-MS) analysis. The total amounts of stigmasterol, β-tocopherol and tocopherol total were highest in the Chia oil obtained by BD, campesterol and sitosterol by SE and γ-tocopherol by SubFE-propane extraction. The SubFE-propane oil also presented the best (2 to 5 times) oxidation stability. SubFE-propane was the most efficient extraction method for Chia oil, providing the highest extraction yields, purity, oxidation stability and diverse profile of sterols.

lipids extraction; fatty acids; subcritical extraction; principal components analysis; phytosterols

Factors	Symbol	Unit	Type	Levels
Factors	Symbol	Unit	Type	-1	0	+1
Temperature	T	°C	Numeric	30	45	60
Pressure	P	MPa	Numeric	8	10	12

Extraction Methods	Temperature / °C	Pressure / MPa	TL / %
A	45	10	28.16^a a Average of triplicates of the center point. Means followed by different italic lowercase letters in the same column demonstrated significant difference by Tukey test (p < 0.05) to different conditions of subcritical extraction chia oil with n-propane. Means followed by different uppercase letters in the same column are significantly different by Tukey test at 5% probability to different methods of chia oil extraction; ^,a,AB
B	30	8	23.61^b b Parameters used in subcritical fluid extraction. ^,b,AB
C	30	12	24.43^b b Parameters used in subcritical fluid extraction. ^,ab,AB
D	60	8	25.77^b b Parameters used in subcritical fluid extraction. ^,ab,AB
E	60	12	27.24^b b Parameters used in subcritical fluid extraction. ^,ab,AB
BD	25	0.1	23.25^B
SE	65	0.1	30.21^A
FLS	25	0.1	27.92^AB

FA	0,0(A)	-1,-1(B)	-1,+1(C)	+1,-1(D)	+1,+1(E)	SE	FLS	BD
16:0	66.01^a ± 2.16	67.59^a ± 2.86	61.57^a ± 1.77	65.60^a ± 6.11	61.93^a ± 0.13	63.08^a ± 0.87	67.76^a ± 8.20	63.57^a ± 0.16
16:1n-9	1.42^ab ± 0.04	1.35^abc ± 0.06	1.37^abc ± 0.05	1.55^a ± 0.22	1.32^abc ± 0.02	1.30^bc ± 0.03	1.16^c ± 0.12	1.37^abc ± 0.01
18:0	27.75^a ± 4.04	25.94^a ± 2.90	23.00^a ± 0.30	24.89^a ± 2.55	23.21^a ± 0.09	23.60^a ± 0.41	26.04^a ± 4.04	23.27^a ± 0.04
18:1n-9 c	56.12^a ± 4.92	60.87^a ± 11.72	50.52^a ± 0.86	53.88^a ± 4.32	50.52^a ± 0.33	51.56^a ± 1.10	67.35^a ± 18.91	53.79^a ± 0.15
18:1n-7	6.97^a ± 0.10	7.24^a ± 0.67	6.78^a ± 0.14	7.21^a ± 0.45	6.93^a ± 0.02	6.84^a ± 0.07	7.09^a ± 0.64	6.91^a ± 0.02
18:2n-6	199.79^a ± 1.11	210.64^a ± 12.10	200.61^a ± 1.34	204.69^a ± 5.86	199.47^a ± 0.16	196.57^a ± 1.28	216.66^a ± 20.95	204.47^a ± 0.19
18:3n-3	611.13^ab ± 11.89	601.75^ab ± 32.04	628.66^a ± 0.71	613.56^ab ± 18.30	626.03^ab ± 1.29	605.35^ab ± 1.53	568.34^b ± 52.58	598.37^ab ± 0.16
24:0	0.56^bc ± 0.03	0.58^b ± 0.02	0.53^bc ± 0.02	0.54^bc ± 0.01	0.58^b ± 0.02	0.68^a ± 0.08	0.48^c ± 0.04	0.72^a ± 0.01
SFA	94.32^a ± 4.58	94.11^a ± 4.08	85.10 ^a ± 1.80	91.04 ^a ± 6.52	85.71^a ± 0.16	87.36 ^a ± 0.96	94.28 ^a ± 9.14	87.56 ^a ± 0.17
MUFA	64.51 ^a ± 4.93	69.46 ^a ± 11.74	58.67 ^a ± 0.88	62.64 ^a ± 4.35	58.77 ^a ± 0.33	59.70 ^a ± 1.10	75.60 ^a ± 18.92	62.06 ^a ± 0.15
PUFA	810.91^a ± 11.94	812.39 ^a ± 34.25	829.27 ^a ± 1.52	818.26 ^a ± 19.22	825.50 ^a ± 1.30	801.92 ^a ± 2.00	785.00 ^a ± 56.60	802.85 ^a ± 0.25
n-3	611.13^ab ± 11.89 601.75 ^ab ± 32.04		628.66^a ± 0.71	613.56 ^ab ± 18.30	626.03 ^ab ± 1.29	605.35 ^ab ± 1.53	568.34^b ± 52.58	598.37 ^ab ± 0.16
n-6	199.79 ^a ± 1.11	210.64 ^a ± 12.10	200.61 ^a ± 1.34	204.69 ^a ± 5.86	199.47 ^a ± 0.16	196.57 ^a ± 1.28	216.66 ^a ± 20.95	204.47 ^a ± 0.19
n-6/n-3	0.33 ^a ± 0.02	0.35^a ± 0.08	0.32 ^a ± 0.01	0.33 ^a ± 0.04	0.32 ^a ± 0.01	0.32 ^a ± 0.01	0.38 ^a ± 0.13	0.34 ^a ± 0.01

Method	Tocopherol		Phytosterol
Method	β-Tocopherol	γ-Tocopherol	Campesterol	Stigmasterol	Sitosterol
A	7.751^e ± 0.511	7.282^a ± 0.245	17.724^f ± 0.799	10.818^f ± 0.888	132.592^f ± 5.194
B	11.262^d ± 1.521	6.638^a ± 0.550	20.279^ef ± 1.254	12.961^ef ± 0.875	151.210^e ± 5.045
C	20.478^c ± 0.290	2.924^b ± 0.197	22.269^de ± 1.676	13.592^def ± 0.702	154.386^de ± 7.130
D	25.693^a ± 0.598	1.121^c ± 0.373	27.072^cd ± 2.248	17.267^bcd ± 0.431	182.863^c ± 7.384
E	23.305^b ± 0.604	2.711^b ± 0.863	24.705^de ± 1.389	16.485* ± 1.965	170.147^c ± 3.713
SE	12.460" ± 0.749	2.341^b ± 0.227	37.190^a ± 1.021	20.125^bc ± 0.681	272.303^a ± 6.880
FLS	22.821^b ± 0.790	n.d.	23.323^cde ± 1.241	20.602^b ± 3.045	168.503^cd ± 0.836
BD	27.304^a ± 0.446	n.d.	30.191^b ± 1.112	25.064^a ± 0.688	218.996^b ± 1.927

	Temperature / ºC
Extraction method	110	120	140	Regression equation	R²
	DSC T₀ / min
A	49.4	25.5	11.3	T = 461.82 - 47.19 log₁₀T₀	0.9661
FLS	27.0	10.8	2.3	T = 423.53 - 28.46 log₁₀T₀	0.9953
BD	31.3	16.4	4.5	T = 432.74 - 33.18 log₁₀T₀	0.9612
SE	38.3	17.7	5.0	T = 436.18 - 33.88 log₁₀T₀	0.9951

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