Analysis of nine antioxidants in vegetable oils by high performance liquid chromatography

doi:10.3724/SP.J.1123.2019.11023

Abstract

Abstract:

A method was developed for the determination of nine antioxidants in vegetable oils by high performance liquid chromatography (HPLC). The samples were extracted with methanol, and the fat in the samples was degreased by freezing. Separation of the targeted compounds was performed on an XBridge C₁₈ column in gradient elution mode using methanol-0.1% (v/v) formic acid aqueous solution as the mobile phase. The analytes were detected using a diode-array detector by the external standard method. The stability and storage conditions for the nine antioxidants were systematically investigated. Ascorbyl palmitate (AP) was introduced into the preparation and pre-treatment of the targets. The concentration of AP was optimized to improve the stability and recovery of the targets. The effects of different extraction solvents and purification methods on the extraction efficiencies were discussed. The results showed that the nine antioxidants could be separated well under the optimized conditions. Good linear relationships in the linear range were obtained, and the correlation coefficients (R²) were greater than 0.999. The average recoveries of the nine antioxidants ranged from 85.3% to 104.1%, with RSDs of the method ≤5.0%. The limits of quantitation (LOQs) for the nine synthetic antioxidants were in the range of 0.6-3.0 mg/kg. The method is simple, rapid, sensitive, and it shows good recovery and reproducibility.

Key words: high performance liquid chromatography (HPLC), ascorbyl palmitate (AP), antioxidants, vegetable oils, stability

ZHAO Huinan, ZHANG Yanxia, XUE Xia, DAI Kun, ZHENG Wenjing, MA Cheng, ZHU Jianhua, LIU Yanming, ZHANG Feng. Analysis of nine antioxidants in vegetable oils by high performance liquid chromatography[J]. Chinese Journal of Chromatography, 2020, 38(7): 841-846.

Figures/Tables 7

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Compound	Linear equation	R²	LOD/ (mg/kg)	LOQ/ (mg/kg)
Y: peak area; X: mass concentration, μg/mL.
PG	Y=0.3083X-0.1720	0.9999	0.2	0.6
THBP	Y=0.2719X-0.8881	0.9991	0.2	0.6
TBHQ	Y=0.0361X+0.0500	0.9996	1.0	3.0
NDGA	Y=0.1074X-0.1052	0.9998	0.5	1.5
BHA	Y=0.0813X-0.0322	0.9999	0.5	1.5
Ionox-100	Y=0.0316X-0.0145	0.9999	1.0	3.0
OG	Y=0.2124X-0.1077	0.9999	0.3	0.8
BHT	Y=0.0502X-0.0145	0.9999	0.8	2.5
DG	Y=0.1790X-0.1057	0.9999	0.3	0.8

Compound	Linear equation	R²	LOD/ (mg/kg)	LOQ/ (mg/kg)
Y: peak area; X: mass concentration, μg/mL.
PG	Y=0.3083X-0.1720	0.9999	0.2	0.6
THBP	Y=0.2719X-0.8881	0.9991	0.2	0.6
TBHQ	Y=0.0361X+0.0500	0.9996	1.0	3.0
NDGA	Y=0.1074X-0.1052	0.9998	0.5	1.5
BHA	Y=0.0813X-0.0322	0.9999	0.5	1.5
Ionox-100	Y=0.0316X-0.0145	0.9999	1.0	3.0
OG	Y=0.2124X-0.1077	0.9999	0.3	0.8
BHT	Y=0.0502X-0.0145	0.9999	0.8	2.5
DG	Y=0.1790X-0.1057	0.9999	0.3	0.8

Compound	Spiked/(mg/kg)	Peanut oil		Soybean oil
Compound	Spiked/(mg/kg)	Recoveries/%	RSDs/%	Recoveries/%	RSDs/%
PG	3.0, 15.0, 50.0	98.3, 96.9, 100.5	1.4, 2.2, 0.7	95.4, 95.8, 102.5	5.0, 2.1, 0.5
THBP	3.0, 15.0, 50.0	94.5, 96.1, 100.6	0.7, 1.1, 0.8	91.8, 95.0, 104.1	4.5, 2.2, 0.6
TBHQ	3.0, 15.0, 50.0	89.0, 90.0, 85.3	1.8, 1.9, 1.0	91.5, 89.8, 99.1	1.8, 0.5, 0.3
NDGA	3.0, 15.0, 50.0	93.5, 95.2, 99.9	3.5, 1.0, 1.3	92.6, 93.4, 102.2	4.0, 1.5, 0.4
BHA	3.0, 15.0, 50.0	97.7, 94.0, 99.3	2.3, 2.6, 0.6	94.3, 95.3, 99.9	4.3, 1.4, 0.4
Ionox-100	3.0, 15.0, 50.0	93.2, 96.1, 101.0	3.2, 0.8, 2.1	93.3, 96.5, 102.1	1.8, 1.8, 0.6
OG	3.0, 15.0, 50.0	94.1, 97.0, 101.9	1.5, 2.4, 0.7	92.3, 96.5, 102.9	1.8, 1.8, 0.3
BHT	3.0, 15.0, 50.0	90.3, 89.9, 88.8	3.0, 1.2, 0.6	90.4, 89.9, 86.1	3.3, 1.7, 1.2
DG	3.0, 15.0, 50.0	94.8, 93.3, 96.6	2.9, 1.0, 0.8	96.3, 94.6, 99.8	2.7, 1.7, 0.6

Compound	Spiked/(mg/kg)	Peanut oil		Soybean oil
Compound	Spiked/(mg/kg)	Recoveries/%	RSDs/%	Recoveries/%	RSDs/%
PG	3.0, 15.0, 50.0	98.3, 96.9, 100.5	1.4, 2.2, 0.7	95.4, 95.8, 102.5	5.0, 2.1, 0.5
THBP	3.0, 15.0, 50.0	94.5, 96.1, 100.6	0.7, 1.1, 0.8	91.8, 95.0, 104.1	4.5, 2.2, 0.6
TBHQ	3.0, 15.0, 50.0	89.0, 90.0, 85.3	1.8, 1.9, 1.0	91.5, 89.8, 99.1	1.8, 0.5, 0.3
NDGA	3.0, 15.0, 50.0	93.5, 95.2, 99.9	3.5, 1.0, 1.3	92.6, 93.4, 102.2	4.0, 1.5, 0.4
BHA	3.0, 15.0, 50.0	97.7, 94.0, 99.3	2.3, 2.6, 0.6	94.3, 95.3, 99.9	4.3, 1.4, 0.4
Ionox-100	3.0, 15.0, 50.0	93.2, 96.1, 101.0	3.2, 0.8, 2.1	93.3, 96.5, 102.1	1.8, 1.8, 0.6
OG	3.0, 15.0, 50.0	94.1, 97.0, 101.9	1.5, 2.4, 0.7	92.3, 96.5, 102.9	1.8, 1.8, 0.3
BHT	3.0, 15.0, 50.0	90.3, 89.9, 88.8	3.0, 1.2, 0.6	90.4, 89.9, 86.1	3.3, 1.7, 1.2
DG	3.0, 15.0, 50.0	94.8, 93.3, 96.6	2.9, 1.0, 0.8	96.3, 94.6, 99.8	2.7, 1.7, 0.6

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