Chinese Journal of Chromatography ›› 2020, Vol. 38 ›› Issue (5): 595-599.DOI: 10.3724/SP.J.1123.2019.09011
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SHEN Weijian(), WANG Hong, LU Huiyuan, YU Keyao, HU Guoshen, WEI Xueyuan, WU Bin
Received:
2019-09-09
Online:
2020-05-08
Published:
2020-12-10
Contact:
SHEN Weijian
Supported by:
SHEN Weijian, WANG Hong, LU Huiyuan, YU Keyao, HU Guoshen, WEI Xueyuan, WU Bin. Determination of eight vitamin E in vegetable oils by gas chromatography-mass spectrometry and its application on authentication of sesame oil[J]. Chinese Journal of Chromatography, 2020, 38(5): 595-599.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2019.09011
Compound | RT/min | RT window/min | Monitoring ions (m/z) |
* Quantitative ion. | |||
δ-T | 8.81 | 6.00-9.10 | 137, 177, 402* |
β-T | 9.34 | 9.10-9.80 | 151, 191, 416* |
γ-T | 9.46 | 9.10-9.80 | 151, 191, 416* |
δ-T3 | 9.53 | 9.10-9.80 | 137, 177, 396* |
α-T | 10.03 | 9.80-10.70 | 165, 205, 430* |
β-T3 | 10.20 | 9.80-10.70 | 151, 191, 410* |
γ-T3 | 10.35 | 9.80-10.70 | 151, 191, 410* |
α-T3 | 11.07 | 10.70-14.00 | 165, 205, 424* |
Table 1 Retention times (RTs), RT windows, and monitoring ions of the eight vitamins E
Compound | RT/min | RT window/min | Monitoring ions (m/z) |
* Quantitative ion. | |||
δ-T | 8.81 | 6.00-9.10 | 137, 177, 402* |
β-T | 9.34 | 9.10-9.80 | 151, 191, 416* |
γ-T | 9.46 | 9.10-9.80 | 151, 191, 416* |
δ-T3 | 9.53 | 9.10-9.80 | 137, 177, 396* |
α-T | 10.03 | 9.80-10.70 | 165, 205, 430* |
β-T3 | 10.20 | 9.80-10.70 | 151, 191, 410* |
γ-T3 | 10.35 | 9.80-10.70 | 151, 191, 410* |
α-T3 | 11.07 | 10.70-14.00 | 165, 205, 424* |
Compound | Linear equation | r | LOD/ (mg/kg) | LOQ/ (mg/kg) |
Y: peak area of quantitative ion; X: mass concentration, mg/L. | ||||
δ-T | Y=42554X-69.713 | 0.9997 | 0.03 | 0.10 |
β-T | Y=49282X-76.982 | 0.9995 | 0.05 | 0.17 |
γ-T | Y=47434X-215.47 | 0.9993 | 0.03 | 0.10 |
δ-T3 | Y=15776X+5.9508 | 0.9996 | 0.15 | 0.50 |
α-T | Y=51856X-506.92 | 0.9967 | 0.08 | 0.27 |
β-T3 | Y=34969X-124.86 | 0.9994 | 0.07 | 0.23 |
γ-T3 | Y=13774X+20.720 | 0.9998 | 0.25 | 0.83 |
α-T3 | Y=23791X-75.181 | 0.9995 | 0.15 | 0.50 |
Table 2 Linear equations, correlation coefficients (r), LODs and LOQs of the eight vitamin E
Compound | Linear equation | r | LOD/ (mg/kg) | LOQ/ (mg/kg) |
Y: peak area of quantitative ion; X: mass concentration, mg/L. | ||||
δ-T | Y=42554X-69.713 | 0.9997 | 0.03 | 0.10 |
β-T | Y=49282X-76.982 | 0.9995 | 0.05 | 0.17 |
γ-T | Y=47434X-215.47 | 0.9993 | 0.03 | 0.10 |
δ-T3 | Y=15776X+5.9508 | 0.9996 | 0.15 | 0.50 |
α-T | Y=51856X-506.92 | 0.9967 | 0.08 | 0.27 |
β-T3 | Y=34969X-124.86 | 0.9994 | 0.07 | 0.23 |
γ-T3 | Y=13774X+20.720 | 0.9998 | 0.25 | 0.83 |
α-T3 | Y=23791X-75.181 | 0.9995 | 0.15 | 0.50 |
Compound | Spiked level/ (mg/kg) | Background/ (mg/kg) | Detected/ (mg/kg) | Average recovery/ % | RSD/ % |
ND: below LOD. | |||||
δ-T | 10 | 13.48 | 22.32 | 88.4 | 6.2 |
50 | 62.68 | 98.4 | 4.8 | ||
250 | 251.28 | 95.1 | 5.3 | ||
β-T | 10 | 0.45 | 10.97 | 105.2 | 4.3 |
50 | 51.65 | 102.4 | 5.2 | ||
250 | 249.35 | 99.6 | 4.9 | ||
γ-T | 10 | 368.91 | 378.54 | 96.3 | 6.5 |
50 | 415.61 | 93.4 | 5.8 | ||
250 | 596.61 | 91.1 | 3.8 | ||
δ-T3 | 10 | ND | 10.62 | 106.2 | 6.0 |
50 | 48.60 | 97.2 | 6.5 | ||
250 | 218.80 | 87.5 | 7.3 | ||
α-T | 10 | 10.46 | 20.09 | 96.3 | 7.2 |
50 | 57.36 | 93.8 | 5.9 | ||
250 | 244.56 | 93.6 | 6.7 | ||
β-T3 | 10 | ND | 10.22 | 102.2 | 7.5 |
50 | 53.70 | 107.4 | 5.5 | ||
250 | 263.20 | 105.3 | 6.6 | ||
γ-T3 | 10 | ND | 9.15 | 91.5 | 4.8 |
50 | 51.60 | 103.2 | 5.6 | ||
250 | 235.50 | 94.2 | 6.9 | ||
α-T3 | 10 | ND | 10.34 | 103.4 | 7.3 |
50 | 52.90 | 105.8 | 6.3 | ||
250 | 241.60 | 96.6 | 6.8 |
Table 3 Average spiked recoveries and RSDs of the eight vitamin E in sesame oil (n=6)
Compound | Spiked level/ (mg/kg) | Background/ (mg/kg) | Detected/ (mg/kg) | Average recovery/ % | RSD/ % |
ND: below LOD. | |||||
δ-T | 10 | 13.48 | 22.32 | 88.4 | 6.2 |
50 | 62.68 | 98.4 | 4.8 | ||
250 | 251.28 | 95.1 | 5.3 | ||
β-T | 10 | 0.45 | 10.97 | 105.2 | 4.3 |
50 | 51.65 | 102.4 | 5.2 | ||
250 | 249.35 | 99.6 | 4.9 | ||
γ-T | 10 | 368.91 | 378.54 | 96.3 | 6.5 |
50 | 415.61 | 93.4 | 5.8 | ||
250 | 596.61 | 91.1 | 3.8 | ||
δ-T3 | 10 | ND | 10.62 | 106.2 | 6.0 |
50 | 48.60 | 97.2 | 6.5 | ||
250 | 218.80 | 87.5 | 7.3 | ||
α-T | 10 | 10.46 | 20.09 | 96.3 | 7.2 |
50 | 57.36 | 93.8 | 5.9 | ||
250 | 244.56 | 93.6 | 6.7 | ||
β-T3 | 10 | ND | 10.22 | 102.2 | 7.5 |
50 | 53.70 | 107.4 | 5.5 | ||
250 | 263.20 | 105.3 | 6.6 | ||
γ-T3 | 10 | ND | 9.15 | 91.5 | 4.8 |
50 | 51.60 | 103.2 | 5.6 | ||
250 | 235.50 | 94.2 | 6.9 | ||
α-T3 | 10 | ND | 10.34 | 103.4 | 7.3 |
50 | 52.90 | 105.8 | 6.3 | ||
250 | 241.60 | 96.6 | 6.8 |
Compound | Sesame oil (n=15) | Soybean oil (n=10) | Rapeseed oil (n=10) | Sunflower oil (n=10) | Peanut oil (n=10) | Maize oil (n=10) | Palm oil (n=10) |
δ-T | 14.54 | 253.42 | 16.47 | 0.60 | 10.31 | 32.08 | ND |
β-T | 0.31 | 25.92 | 3.16 | 20.33 | 6.59 | 11.23 | 1.71 |
γ-T | 447.83 | 739.42 | 370.89 | 7.70 | 98.50 | 522.53 | 3.57 |
α-T | 8.56 | 167.95 | 247.07 | 527.70 | 152.45 | 180.88 | 170.56 |
δ-T3 | ND | ND | ND | ND | ND | ND | 86.62 |
β-T3 | ND | ND | ND | ND | ND | ND | 15.00 |
γ-T3 | ND | ND | ND | ND | ND | 16.38 | 337.74 |
α-T3 | ND | ND | ND | ND | ND | 11.54 | 218.06 |
Table 4 Contents of tocopherols and tocotrienols in vegetable oils mg/kg
Compound | Sesame oil (n=15) | Soybean oil (n=10) | Rapeseed oil (n=10) | Sunflower oil (n=10) | Peanut oil (n=10) | Maize oil (n=10) | Palm oil (n=10) |
δ-T | 14.54 | 253.42 | 16.47 | 0.60 | 10.31 | 32.08 | ND |
β-T | 0.31 | 25.92 | 3.16 | 20.33 | 6.59 | 11.23 | 1.71 |
γ-T | 447.83 | 739.42 | 370.89 | 7.70 | 98.50 | 522.53 | 3.57 |
α-T | 8.56 | 167.95 | 247.07 | 527.70 | 152.45 | 180.88 | 170.56 |
δ-T3 | ND | ND | ND | ND | ND | ND | 86.62 |
β-T3 | ND | ND | ND | ND | ND | ND | 15.00 |
γ-T3 | ND | ND | ND | ND | ND | 16.38 | 337.74 |
α-T3 | ND | ND | ND | ND | ND | 11.54 | 218.06 |
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