Development of a Simultaneous Normal-Phase HPLC Analysis of Lignans, Tocopherols, Phytosterols, and Squalene in Sesame Oil Samples
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals
2.2. Sesame Oil Samples
2.3. Sample Preparation
2.4. HPLC-DAD-FLD Analysis
2.5. Method Validation
2.6. Statistical Analysis
3. Results
3.1. Development of Simultaneous Determination of Lignans, Tocopherols, Phytosterols, and Squalene
3.2. Method Validation
3.2.1. Linearity, LOD, and LOQ
3.2.2. Precision and Accuracy
3.2.3. Recovery
3.3. Analysis of Lignans, Tocopherols, Squalene, and Phytosterol in Sesame Oil Samples
3.4. Statistical Analysis of Principal Component Analysis (PCA)
4. Conclusions
Supplementary Materials
Author Contributions
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Abbreviations
CPO | Cold-pressed sesame oil |
DAD | Diode array detector |
FLD | Fluorescence detector |
HPLC | High-performance liquid chromatography |
LOD | Limit of detection |
LOQ | Limit of quantification |
MSCO | Sesame cooking oil mixed with other oil |
NP | Normal-phase |
PCA | Principal component analysis |
RP | Reverse-phase |
RSDs | Relative standard deviations |
SCO | Sesame cooking oil |
SOS | Sesame oil supplement |
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Compounds | Retention Time (min) | Regression Equation | Correlation (R2) | LOD a (µg mL−1) | LOQ b (µg mL−1) |
---|---|---|---|---|---|
Sesamin | 10.34 | y = 36.705x − 2.918 | 0.9982 | 0.02 | 0.05 |
Sesamolin | 8.94 | y =26.738x + 19.573 | 0.9901 | 0.10 | 0.12 |
Sesamol | 11.73 | y = 46.016x + 13.691 | 0.9975 | 0.02 | 0.04 |
Asarinin | 9.08 | y = 30.685x + 5.4833 | 0.9947 | 0.10 | 0.12 |
α-Tocopherol | 6.31 | y = 21.621x − 6.6543 | 0.9996 | 0.41 | 0.43 |
β-Tocopherol | 6.97 | y = 41.061x + 3.1872 | 0.9998 | 0.35 | 0.42 |
γ-Tocopherol | 7.52 | y = 44.828x + 3.2547 | 0.9999 | 0.40 | 0.42 |
δ-Tocopherol | 8.44 | y = 43.128x + 15.908 | 0.9995 | 0.21 | 0.40 |
Phytosterols | 18.17 | y = 6.2278x + 60.16 | 0.9992 | 10.04 | 10.34 |
Squalene | 7.38 | y = 0.0453x − 5.2587 | 0.9986 | 307.07 | 326.23 |
Compounds | Concentration (µg mL−1) | Intra-Day %RSD (n = 6) | Inter-Day %RSD (n = 3) | Recovery (%) |
---|---|---|---|---|
Sesamin | Con 1 | 0.18 | 0.61 | 107.2 |
Con 2 | 1.09 | 3.07 | 100.4 | |
Con 3 | 0.78 | 3.02 | 104.8 | |
Sesamolin | Con 1 | 0.14 | 0.66 | 99.3 |
Con 2 | 0.35 | 1.39 | 100.2 | |
Con 3 | 0.27 | 3.32 | 97.8 | |
Sesamol | Con 1 | 0.04 | 0.22 | 91.6 |
Con 2 | 0.14 | 0.39 | 102.8 | |
Con 3 | 0.27 | 0.14 | 88.4 | |
Asarinin | Con 1 | 0.12 | 0.40 | 101.1 |
Con 2 | 0.42 | 1.46 | 99.7 | |
Con 3 | 0.46 | 2.65 | 93.5 | |
α-Tocopherol | Con 1 | 0.27 | 0.03 | 92.5 |
Con 2 | 0.16 | 0.45 | 88.9 | |
Con 3 | 0.33 | 0.26 | 96.7 | |
β-Tocopherol | Con 1 | 0.28 | 0.10 | 102.0 |
Con 2 | 0.22 | 0.25 | 109.4 | |
Con 3 | 0.30 | 0.36 | 113.5 | |
γ-Tocopherol | Con 1 | 0.08 | 0.35 | 100.0 |
Con 2 | 0.12 | 0.34 | 98.5 | |
Con 3 | 0.19 | 0.33 | 107.6 | |
δ-Tocopherol | Con 1 | 0.07 | 0.11 | 102.6 |
Con 2 | 0.07 | 0.13 | 90.6 | |
Con 3 | 0.16 | 0.34 | 91.4 | |
Squalene | Con 1 | 0.04 | 0.30 | 99.7 |
Con 2 | 0.10 | 0.28 | 100.9 | |
Con 3 | 0.22 | 0.46 | 104.7 | |
Phytosterol | Con 1 | 0.01 | 0.10 | 91.0 |
Con 2 | 0.04 | 0.13 | 92.5 | |
Con 3 | 0.03 | 0.25 | 94.6 |
Sample | Tocopherol | Lignan | Squalene | Phytosterols | ||||||
---|---|---|---|---|---|---|---|---|---|---|
α-T a | β-T | γ-T | δ-T | Sesamolin | Asarinin | Sesamin | Sesamol | |||
CPO-1 | ND b | ND | 293.8 | ND | 2240 | ND | 2315 | ND | 875 | 6640 |
CPO-2 | ND | ND | 286.6 | ND | 1275 | ND | 1260 | ND | 935 | 6385 |
CPO-3 | ND | ND | 377.5 | ND | 1540 | ND | 1480 | ND | 1005 | 6690 |
CPO-4 | ND | ND | 298.9 | ND | 1300 | ND | 1280 | ND | 960 | 6530 |
CPO-5 | ND | ND | 324.8 | ND | 1645 | ND | 1620 | ND | 1030 | 6610 |
CPO-6 | ND | ND | 194.2 | ND | 2800 | ND | 2990 | ND | 845 | 9500 |
CPO-7 | ND | ND | 169.4 | ND | 1820 | ND | 1940 | ND | 910 | 5065 |
SOS-1 | ND | ND | 162.0 | 1.3 | 1630 | ND | 1630 | ND | 4030 | 4885 |
SOS-2 | ND | ND | 249.4 | ND | 3330 | ND | 3840 | ND | 995 | 5490 |
SOS-3 | ND | ND | 29.7 | ND | 3000 | ND | 3540 | ND | 245 | 7055 |
SOS-4 | ND | ND | 266.9 | ND | 4240 | ND | 4725 | ND | 1195 | 6725 |
SCO-1 | 38.3 | 5.4 | 298.8 | ND | 2130 | 92.8 | 2495 | 7.6 | 875 | 4120 |
SCO-2 | ND | ND | 391.6 | ND | 2615 | 122.8 | 3215 | 25.1 | 965 | 7020 |
SCO-3 | ND | ND | 329.2 | ND | 2365 | 115.2 | 2690 | 9.5 | 990 | 6900 |
SCO-4 | ND | ND | 250.9 | ND | 2175 | 168.9 | 2740 | 7.9 | 815 | 4560 |
SCO-5 | ND | ND | 254.1 | ND | 2500 | 41.8 | 2900 | 5.5 | 905 | 5850 |
SCO-6 | ND | ND | 275.3 | ND | 2850 | 132.9 | 3360 | 121.5 | 1040 | 5210 |
SCO-7 | 147.8 | ND | 226.4 | ND | 1730 | 323.8 | 4360 | 30.5 | 620 | 3930 |
SCO-8 | ND | ND | 400.7 | ND | 2300 | 157.8 | 2740 | 30.0 | 990 | 5495 |
SCO-9 | ND | ND | 307.5 | ND | 1500 | 18.0 | 2980 | 42.8 | 1260 | 4610 |
SCO-10 | ND | ND | 270.0 | ND | 2140 | 126.1 | 2440 | 20.4 | 990 | 4835 |
SCO-11 | ND | ND | 283.0 | ND | 2860 | 60.3 | 3180 | 105.3 | 1050 | 5895 |
SCO-12 | 80.0 | 18.9 | 206.7 | ND | 1490 | 12.7 | 2115 | ND | 705 | 4000 |
MSCO-1 | 100.3 | 12.6 | 343.9 | ND | 420 | 145.2 | 1210 | ND | 1160 | 2640 |
MSCO-2 | 53.2 | 14.1 | 311.9 | ND | 1390 | 104.5 | 1765 | 32.0 | 1115 | 4195 |
MSCO-3 | 139.4 | 18.8 | 529.7 | ND | 685 | 213.1 | 1555 | 1.7 | 1175 | 3640 |
MSCO-4 | 57.2 | 21.8 | 308.7 | ND | 1800 | 150.4 | 2525 | 7.8 | 1070 | 3995 |
MSCO-5 | 67.8 | 14.7 | 357.9 | ND | 1215 | 183.5 | 1515 | 30.6 | 1130 | 3090 |
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Yuenyong, J.; Bennett, C.; Jiamyangyuen, S.; Mahatheeranont, S.; Sookwong, P. Development of a Simultaneous Normal-Phase HPLC Analysis of Lignans, Tocopherols, Phytosterols, and Squalene in Sesame Oil Samples. Foods 2024, 13, 1368. https://doi.org/10.3390/foods13091368
Yuenyong J, Bennett C, Jiamyangyuen S, Mahatheeranont S, Sookwong P. Development of a Simultaneous Normal-Phase HPLC Analysis of Lignans, Tocopherols, Phytosterols, and Squalene in Sesame Oil Samples. Foods. 2024; 13(9):1368. https://doi.org/10.3390/foods13091368
Chicago/Turabian StyleYuenyong, Jitkunya, Chonlada Bennett, Sudarat Jiamyangyuen, Sugunya Mahatheeranont, and Phumon Sookwong. 2024. "Development of a Simultaneous Normal-Phase HPLC Analysis of Lignans, Tocopherols, Phytosterols, and Squalene in Sesame Oil Samples" Foods 13, no. 9: 1368. https://doi.org/10.3390/foods13091368