Process optimization and oxidative stability analysis of Camellia oleifera seed oil via supercritical carbon dioxide extraction

doi:10.3969/j.issn.1004-1524.20250542

Acta Agriculturae Zhejiangensis ›› 2026, Vol. 38 ›› Issue (6): 1141-1152.DOI: 10.3969/j.issn.1004-1524.20250542

• Future Foods and Health • Previous Articles Next Articles

Process optimization and oxidative stability analysis of Camellia oleifera seed oil via supercritical carbon dioxide extraction

LI Peng¹(), ZHAN Xi², ZHANG Hui¹^,^*()

¹ College of Biosystems Engineering and Food Science, Zhejiang University, Hangzhou 310058, China
² Zhejiang Publishing United Group, Hangzhou 310006, China

Received:2025-08-14 Online:2026-06-25 Published:2026-07-14

Abstract

Abstract:

Camellia oleifera seed oil, a unique woody oil native to China, is rich in various nutrients and bioactive compounds and is widely used in the food, cosmetic and pharmaceutical industries. Efficient extraction of high-quality C. oleifera seed oil is a key prerequisite for its high-value utilization. Based on the properties of supercritical fluids, this study used a central composite design-response surface methodology (CCD-RSM) to systematically investigate the effects of temperature (35-95 ℃), pressure (8-40 MPa), equilibration time (10-50 min) and extraction time (12-60 min) on oil yield, as well as on the contents of squalene and triterpene alcohols in the oil during supercritical carbon dioxide (SC-CO₂) extraction. A second-order polynomial regression model of the independent variables was established to predict the optimal process conditions, and the chemical composition and antioxidant capacity of the oil obtained under the optimal conditions were analyzed. Three optimal conditions were derived from the prediction model: Y1 (temperature 75 ℃, pressure 35.2 MPa, equilibration time 25.5 min, extraction time 50.2 min) for maximizing oil yield; Y2 (temperature 55 ℃, pressure 20.4 MPa, equilibration time 38.8 min, extraction time 14.3 min) for maximizing squalene content; and Y3 (temperature 70 ℃, pressure 10.8 MPa, equilibration time 19.9 min, extraction time 41.1 min) for maximizing triterpene alcohol content. Under different extraction conditions, significant differences were observed in oil yield, squalene content, triterpene alcohol content and antioxidant capacity, whereas the fatty acid composition remained largely similar. The measured values under the optimal conditions were in good agreement with the model predictions: oil yield under Y1 was 23.96% (mass fraction), squalene content under Y2 was 288.89 mg·kg^-1, and triterpene alcohol content under Y3 was 2 283.50 mg·kg^-1. This study confirms that supercritical fluid extraction can selectively enhance the levels of bioactive compounds in C. oleifera seed oil, providing a theoretical reference and practical support for obtaining high-quality oil and promoting its high-value applications.

Key words: Camellia oleifera seed oil, supercritical carbon dioxide extraction, response surface methodology, chemical composition, antioxidant capacity, squalene, triterpene alcohol

CLC Number:

TS224.4

LI Peng, ZHAN Xi, ZHANG Hui. Process optimization and oxidative stability analysis of Camellia oleifera seed oil via supercritical carbon dioxide extraction[J]. Acta Agriculturae Zhejiangensis, 2026, 38(6): 1141-1152.

Figures/Tables 9

References 48

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响应变量 Response variable	F值 F value	p值 p value	R²	调整R² ${\mathit{R}}_{\mathit{a}\mathit{d}\mathit{j}}^{2}$	失拟项p值 p value of lack of fit
产率Yield	34.17	<0.000 1	0.968	0.939	0.173
角鲨烯含量Squalene content	12.21	<0.000 1	0.914	0.840	0.833
三萜烯醇含量Triterpene alcohol content	14.83	<0.000 1	0.928	0.866	0.567

响应变量 Response variable	F值 F value	p值 p value	R²	调整R² ${\mathit{R}}_{\mathit{a}\mathit{d}\mathit{j}}^{2}$	失拟项p值 p value of lack of fit
产率Yield	34.17	<0.000 1	0.968	0.939	0.173
角鲨烯含量Squalene content	12.21	<0.000 1	0.914	0.840	0.833
三萜烯醇含量Triterpene alcohol content	14.83	<0.000 1	0.928	0.866	0.567

响应值 Response value	变量 Variable	回归系数 Regression coefficient	F值 F value	p值 p value
产率Yield	截距Intercept	21.15	—	—
	X₁	0.540 6	13.67	<0.000 1
	X₂	2.65	327.99	0.002 0
	X₃	0.643 0	19.33	<0.000 1
	X₄	0.945 9	41.83	0.000 5
	X₁X₂	0.486 1	7.36	<0.000 1
	${\mathit{X}}_{1}^{2}$	-0.408 5	9.30	0.015 3
	${\mathit{X}}_{2}^{2}$	-1.04	60.59	0.007 7
角鲨烯含量 Squalene content	截距Intercept	224.72	—	—
	X₂	-12.09	17.76	<0.000 1
	X₄	-27.17	89.68	<0.000 1
	X₁X₂	-9.56	7.41	0.015 1
	X₁X₃	-12.99	13.66	0.002 0
	X₁X₄	8.13	5.36	0.034 2
	${\mathit{X}}_{1}^{2}$	-10.41	15.70	0.001 1
	${\mathit{X}}_{2}^{2}$	-9.78	13.85	0.001 9
三萜烯醇含量 Triterpene alcohol content	截距Intercept	2 001.86	—	—
	X₂	-76.09	14.83	<0.000 1
	X₁X₂	28.86	94.61	0.008 3
	X₁X₃	-27.65	9.07	0.010 7
	X₁X₄	26.28	8.33	0.014 4
	X₂X₃	65.90	7.53	<0.000 1
	${\mathit{X}}_{1}^{2}$	-29.45	47.31	0.000 8
	${\mathit{X}}_{2}^{2}$	-20.88	16.88	0.010 2
	${\mathit{X}}_{4}^{2}$	-28.68	8.48	0.001 0

响应值 Response value	变量 Variable	回归系数 Regression coefficient	F值 F value	p值 p value
产率Yield	截距Intercept	21.15	—	—
	X₁	0.540 6	13.67	<0.000 1
	X₂	2.65	327.99	0.002 0
	X₃	0.643 0	19.33	<0.000 1
	X₄	0.945 9	41.83	0.000 5
	X₁X₂	0.486 1	7.36	<0.000 1
	${\mathit{X}}_{1}^{2}$	-0.408 5	9.30	0.015 3
	${\mathit{X}}_{2}^{2}$	-1.04	60.59	0.007 7
角鲨烯含量 Squalene content	截距Intercept	224.72	—	—
	X₂	-12.09	17.76	<0.000 1
	X₄	-27.17	89.68	<0.000 1
	X₁X₂	-9.56	7.41	0.015 1
	X₁X₃	-12.99	13.66	0.002 0
	X₁X₄	8.13	5.36	0.034 2
	${\mathit{X}}_{1}^{2}$	-10.41	15.70	0.001 1
	${\mathit{X}}_{2}^{2}$	-9.78	13.85	0.001 9
三萜烯醇含量 Triterpene alcohol content	截距Intercept	2 001.86	—	—
	X₂	-76.09	14.83	<0.000 1
	X₁X₂	28.86	94.61	0.008 3
	X₁X₃	-27.65	9.07	0.010 7
	X₁X₄	26.28	8.33	0.014 4
	X₂X₃	65.90	7.53	<0.000 1
	${\mathit{X}}_{1}^{2}$	-29.45	47.31	0.000 8
	${\mathit{X}}_{2}^{2}$	-20.88	16.88	0.010 2
	${\mathit{X}}_{4}^{2}$	-28.68	8.48	0.001 0

条件 Condition	产率/% Yield/%	角鲨烯含量/ (mg·kg^-1) Squalene content/ (mg·kg^-1)	三萜烯醇含量/ (mg·kg^-1) Triterpene alcohol content/(mg·kg^-1)
Y1	23.96±0.63 a	163.25±6.46 c	1 783.32±15.86 c
Y2	16.32±0.74 b	288.89±6.37 a	1 985.33±6.98 b
Y3	12.64±0.36 c	225.88±9.04 b	2 283.50±22.75 a

Process optimization and oxidative stability analysis of Camellia oleifera seed oil via supercritical carbon dioxide extraction

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水平 Level	变量Variable
水平 Level	X₁/℃	X₂/MPa	X₃/min	X₄/min
-2	35	8	10	12
-1	50	16	20	24
0	65	24	30	36
+1	80	32	40	48
+2	95	40	50	60

实验号 Test number	变量 Variable				产率/% Yield/%	角鲨烯含量/ (mg·kg^-1) Squalene content/ (mg·kg^-1)	三萜烯醇含量/ (mg·kg^-1) Triterpene alcohol content/ (mg·kg^-1)
实验号 Test number	X₁/℃	X₂/MPa	X₃/min	X₄/min	产率/% Yield/%	角鲨烯含量/ (mg·kg^-1) Squalene content/ (mg·kg^-1)	三萜烯醇含量/ (mg·kg^-1) Triterpene alcohol content/ (mg·kg^-1)
1	65	24	30	36	20.02±0.17	278.60±5.02	1 986.71±10.24
2	50	32	20	24	19.68±0.11	302.42±4.99	1 798.62±7.66
3	65	24	30	12	17.44±0.15	337.26±4.34	1 915.35±7.59
4	65	40	30	36	22.86±0.20	221.19±6.09	1 745.68±22.78
5	50	16	40	48	17.93±0.55	245.53±6.99	1 943.53±11.02
6	50	16	20	24	15.96±0.12	312.40±5.67	2 095.02±8.41
7	50	32	40	48	22.23±0.65	247.95±4.77	1 924.05±9.32
8	65	24	30	36	21.52±0.23	282.50±4.30	2 044.01±12.38
9	80	16	20	48	16.53±0.26	297.70±5.19	2 086.06±9.89
10	65	24	30	36	21.50±0.14	312.30±5.25	2 039.44±24.03
11	80	32	40	24	22.27±0.34	276.50±6.40	1 879.04±10.78
12	80	16	20	24	15.15±0.24	343.27±9.56	2 019.08±11.67
13	65	8	30	36	10.72±0.26	266.98±8.01	2 108.32±6.01
14	65	24	50	36	21.77±0.22	268.70±8.48	1 951.43±16.66
15	50	32	40	24	20.30±0.21	277.18±6.09	1 892.65±5.78
16	35	24	30	36	17.72±0.18	238.57±4.75	1 940.16±17.98
17	80	16	40	48	18.65±0.44	284.72±5.49	1 860.19±9.67
18	80	16	40	24	16.47±0.35	314.58±4.32	1 832.45±7.69
19	80	32	20	48	23.09±0.28	270.30±3.69	1 828.60±8.82
20	95	24	30	36	20.94±0.15	271.15±4.68	1 845.26±10.53
21	80	32	20	24	21.66±0.45	283.95±9.76	1 824.33±6.18
22	65	24	30	60	22.63±0.08	266.53±3.66	1 876.26±14.16
23	65	24	30	36	21.53±0.37	292.30±4.90	1 994.05±7.72
24	65	24	30	36	21.04±0.60	277.50±6.49	1 927.08±18.53
25	65	24	10	36	17.97±0.12	324.22±4.56	2 047.35±6.97
26	65	24	30	36	21.39±0.51	300.80±7.05	2 007.66±12.92
27	50	16	40	24	16.43±0.15	284.57±9.56	2 029.05±21.91
28	80	32	40	48	23.51±0.11	256.63±5.93	1 946.21±10.58
29	50	16	20	48	17.12±0.16	270.20±5.15	2 011.22±6.01
30	65	24	30	36	21.03±0.18	314.60±4.41	2 014.10±8.95
31	50	32	20	48	21.18±0.24	268.88±3.81	1 682.15±9.73

条件 Conditions	脂肪酸组分含量/%Contents of fatty acid composition/%													α-生育酚含量/ (mg·kg^-1) α-Tocopherol content/ (mg·kg^-1)	多酚含量/ (mg·kg^-1) Polyphenols content/ (mg·kg^-1)
条件 Conditions	C6: 0	C8: 0	C10: 0	C11: 0	C12: 0	C13: 0	C16: 0	C17: 0	C18: 0	C18: 1顺式 C18:1 cis	C18: 2顺式 C18:2 cis	C18: 3n3	C24: 1	α-生育酚含量/ (mg·kg^-1) α-Tocopherol content/ (mg·kg^-1)	多酚含量/ (mg·kg^-1) Polyphenols content/ (mg·kg^-1)
Y1	0.82	0.68	0.65	0.60	0.51	0.51	7.72	6.56	2.15	64.98	6.41	0.69	0.56	125.49±0.75 b	188.50±2.80 b
Y2	0.76	0.64	0.60	0.56	0.47	0.47	7.72	6.15	2.15	66.28	6.39	0.65	0.52	104.37±0.88 c	126.40±1.50 c
Y3	0.73	0.61	0.58	0.53	0.45	0.45	7.73	6.04	2.17	66.74	6.42	0.64	0.50	134.35±0.39 a	229.60±3.30 a

条件 Conditions	DPPH (IC₅₀)/ (g·L^-1)	ABTS (IC₅₀)/ (g·L^-1)	IP/h
Y1	22.65±0.75 b	75.87±1.02 b	12.89±0.32 a
Y2	30.41±0.88 a	94.79±1.35 a	3.73±0.08 c
Y3	29.91±0.39 a	63.57±0.96 c	8.28±0.19 b

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