Simultaneous Determination of Four Fatty Acids in Coix Seeds via Gas Chromatography
Abstract
1. Introduction
2. Materials and Methods
2.1. Instrumentation
2.2. Chemicals and Reagents
2.3. Experimental Materials
2.4. Chromatographic Conditions
2.5. Preparation of the Mixed Reference Solution
2.6. Preparation of the Test Solution
2.7. Data Analysis
3. Results and Discussion
3.1. Chromatographic Conditions Screening
3.2. Standard Curve and Linear Range
3.3. Precision Experiment
3.4. Repeatability Test
3.5. Stability Test
3.6. Spiked Recovery Test
3.7. Testing and Analysis of Samples from Different Origins
3.8. Clustering Analysis
4. Conclusions
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
References
- Li, H.J.; Peng, L.X.; Yin, F.; Fang, J.H.; Cai, L.T.; Zhang, C.J.; Xiang, Z.; Zhao, Y.Y.; Zhang, S.F.; Sheng, H.D.; et al. Research on Coix seed as a food and medicinal resource, it’s chemical components and their pharmacological activities: A review. J. Ethnopharmacol. 2024, 319, 117309. [Google Scholar] [CrossRef]
- Wang, Y.M.; Wu, J.K.; Lian, T.T.; Wang, Y.Y.; Zhang, F.F.; Li, X.; Xu, Y.Y.; Liu, S.Q.; Li, Y.B. Exploring chemical markers and identifying phenolic markers using a metabolomics strategy and chemometrics to study the different origins of defatted Coix seed. Food Res. Int. 2024, 194, 114864. [Google Scholar] [CrossRef] [PubMed]
- Liao, L.; Lin, S.T.; Liang, J.F.; Li, X.; Chen, Y.M.; Ye, L.; Li, J.Y.; Zeng, X.A. Research progress in pharmacologically active ingredients of Coix Seeds as a source of both food and medicine. Food Sci. 2025, 46, 358–367. [Google Scholar] [CrossRef]
- Diao, X. Production and genetic improvement of minor cereals in China. Crop J. 2017, 5, 103–114. [Google Scholar] [CrossRef]
- Zeng, Y.; Yang, J.; Chen, J.; Pu, X.; Li, X.; Yang, X.; Yang, L.; Ding, Y.; Nong, M.; Zhang, S.; et al. Actional mechanisms of active ingredients in functional food adlay for human health. Molecules 2022, 27, 4808. [Google Scholar] [CrossRef] [PubMed]
- Devaraj, R.D.; Jeepipalli, S.P.; Xu, B. Phytochemistry and health promoting effects of Job’s tears (Coix lacrymajobi)—A critical review. Food Biosci. 2020, 34, 100537. [Google Scholar] [CrossRef]
- Nurkolis, F.; Gunawan, W.; Hardinsyah, H.; Mayulu, N.; Wijayanti, M. Health benefits of Coix seed (Coix lacryma-jobi): A study review. Curr. Dev. Nutr. 2022, 6, 524. [Google Scholar] [CrossRef]
- Sui, Y.; Xu, D.; Sun, X. Identification of anti-hyperuricemic components from Coix seed. Food Biosci. 2023, 52, 102461. [Google Scholar] [CrossRef]
- Fu, J.J.; Dong, X.; Zhong, F.X.; Li, X.Y. Nutritional composition and modern pharmacological research progress of Coix Seeds. Sci. Technol. Cereals Oils Foods 2023, 31, 93–95. [Google Scholar] [CrossRef]
- Li, X.D.; Pan, H.; Lu, X.J.; Wie, X.Y.; Lu, P.; Shi, M.; Qin, L.K. Characteristics and comprehensive assessment of principal nutritional components in adlay landraces. Sci. Agric. Sin. 2018, 51, 835–842. [Google Scholar] [CrossRef]
- Li, X.D.; Lu, X.J.; Pan, H.; Wei, X.Y.; Zeng, T.; Guo, C.; Lu, P.; Zhou, M.L.; Gao, A.N.; Shi, M. Classification of principal lipid components and distinctive molecules selection in adlay seed (Coix L.). J. Chin. Cereals Oils Assoc. 2025, 40, 41–48. [Google Scholar] [CrossRef]
- Hou, J.J.; Cao, C.M.; Xu, Y.W.; Yao, S.; Cai, L.Y.; Long, H.L.; Bi, Q.R.; Zhen, Y.Y.; Wu, W.Y.; Guo, D.A. Exploring lipid markers of the quality of coix seeds with different geographical origins using supercritical fluid chromatography mass spectrometry and chemometrics. Phytomedicine 2018, 45, 1–7. [Google Scholar] [CrossRef] [PubMed]
- Li, X.K.; Gu, K.; Liang, M.W.; Zhang, Y.T.; Wang, Y.M.; Li, Y.B. Research progress on chemical constituents and pharmacological effects of Coicis Semen. Chin. Tradit. Herb. Drug 2020, 51, 5645–5657. [Google Scholar] [CrossRef]
- Xi, X.J.; Zhu, Y.G.; Tong, Y.P.; Yang, X.L.; Tang, N.N.; Ma, S.M.; Cheng, Z. Assessment of the genetic diversity of different Job’s tears (Coix lacryma-jobi L.) accessions and the active composition and anticancer effect of its seed oil. PLoS ONE 2016, 11, e0153269. [Google Scholar] [CrossRef]
- Yang, Y.; Du, S.Y.; Sun, Y.Q.; Han, T.; Jia, M.; Qin, L.P. Determination of effective contents triolein and coixol in Coix lacrymajobi var. mayuen from different origins. Chin. Tradit. Herb. Drugs 2017, 48, 578–581. Available online: https://www.tiprpress.com/zcy/html/2017/3/20170325.htm (accessed on 7 September 2025).
- Zhu, W.H.; Du, W.F.; Lou, Y.J.; Hong, H.; Hong, Z.H.; Ge, Z.W.; Li, C.Y.; Ge, W.H. Analysis of chemical constituents of fatty acids and their esters of Coix Seeds by UPLC-Triple-TOF-MS. Chin. Tradit. Herb. Drugs 2020, 51, 3876–3883. [Google Scholar] [CrossRef]
- Huang, Z.Y.; Gutterman, Y.; Osborne, D.J. Value of the mucilaginous pellicle to seeds of the sand-stabilizing desert woody shrub Artemisia sphaerocephala (Asteraceae). Trees 2004, 18, 669–676. [Google Scholar] [CrossRef]
- Li, Y.T.; Hu, C.X.; Chen, X.T.; Qi, Z.B.; Xie, F.; Liu, Q. Fatty acid analysis and detection method of Artemisia sphaerocephala seeds based on GC-MS/MS. Pratacult. Sci. 2025, 42, 786–794. [Google Scholar] [CrossRef]
- Ma, Z.Z.; Li, X.Q.; Huang, M.M.; Wang, F.; Chen, Y. Determination of triglycerides and fatty acids in Coix Seeds from different areas and its quality evaluation. Chin. Tradit. Herb. Drugs 2020, 51, 210–215. [Google Scholar] [CrossRef]
- Zhou, X.; Fan, J.; Xu, B.; Wu, F.Q.; Zhuang, C.H.; Wang, J.F. GC internal standard method simultaneously determines the six fatty acid components in the pollen of Brassica campestis Linn. Chin. Tradit. Pat. Med. 2023, 45, 2760–2763. [Google Scholar] [CrossRef]
- Ye, H.; Li, J.J.; Zheng, B.; Wang, M.; Zhao, M.; Zhao, C.J. Simultaneous determination of four fatty acid component in descuraina semen by GC. J. Shenyang Pharm. Univ. 2020, 37, 246–251. [Google Scholar] [CrossRef]
- Kawajiri, Y. Model-based optimization strategies for chromatographic processes: A review. Adsorption 2021, 27, 1–26. [Google Scholar] [CrossRef]
- Peng, L.; Gao, X.; Wang, L.; Zhu, A.; Cai, X.; Li, P.; Li, W. Design of experiment techniques for the optimization of chromatographic analysis conditions: A review. Electrophoresis 2022, 43, 1882–1898. [Google Scholar] [CrossRef]
- Bártů, V.; Wičar, S. Optimization of temperature programs in gas chromatography. Anal. Chim. Acta 1983, 150, 245–252. [Google Scholar] [CrossRef]
Sample Number | Place of Origin | Sample Number | Place of Origin |
---|---|---|---|
S1 | Chengdu, Sichuan | S13 | Zhangshu, Jiangxi |
S2 | Chengdu, Sichuan | S14 | Zhangshu, Jiangxi |
S3 | Chengdu, Sichuan | S15 | Zhangshu, Jiangxi |
S4 | Chengdu, Sichuan | S16 | Yulin, Guangxi |
S5 | Chengdu, Sichuan | S17 | Yulin, Guangxi |
S6 | Anguo, Hebei | S18 | Yulin, Guangxi |
S7 | Anguo, Hebei | S19 | Yulin, Guangxi |
S8 | Anguo, Hebei | S20 | Yulin, Guangxi |
S9 | Anguo, Hebei | S21 | Guiyang, Guizhou |
S10 | Anguo, Hebei | S22 | Guiyang, Guizhou |
S11 | Zhangshu, Jiangxi | S23 | Guiyang, Guizhou |
S12 | Zhangshu, Jiangxi | S24 | Guiyang, Guizhou |
Condition | Chromatographic Conditions | Result | ||||
---|---|---|---|---|---|---|
T0/°C | t1/min | r (°C/min) | T1/°C | t2/min | ||
1 | 200 | 4 | 5 | 230 | 6 | Chromatographic peaks are not separated. |
2 | 200 | 4 | 3 | 230 | 6 | Chromatographic peaks have tails and are asymmetrical. |
3 | 200 | 4 | 4 | 230 | 6 | Both peak shape and resolution are good. |
4 | 200 | 3 | 4 | 230 | 6 | Both peak shape and resolution are good. |
5 | 220 | 3 | 4 | 230 | 6 | Chromatographic peaks are not separated. |
Fatty Acid | 1 SC | 2 LR/μg/mL | 3 r |
---|---|---|---|
Palmitic acid | Y = 0.8389x−10.516 | 282.50~2825.00 | 1.0000 |
Stearic acid | Y = 1.1369x−64.786 | 262.00~1572.00 | 0.9996 |
Oleic acid | Y = 0.8104x−20.604 | 425.25~2976.75 | 0.9990 |
Linoleic acid | Y = 1.0051x−143.57 | 304.50~1218.00 | 0.9990 |
Fatty Acid | 1 SW (g) | 2 SC (mg) | 3 AV (mg) | 4 AA (mg) | 5 RR% | 6 ARR% | RSD% |
---|---|---|---|---|---|---|---|
Palmitic acid (PA) | P | 0.027 | 0.056 | 0.028 | 101.81 | 99.40 | 3.75 |
0.2500 | 0.027 | 0.055 | 0.028 | 98.23 | |||
0.2499 | 0.027 | 0.055 | 0.028 | 98.27 | |||
0.2502 | 0.028 | 0.054 | 0.028 | 94.56 | |||
0.2499 | 0.027 | 0.057 | 0.028 | 105.42 | |||
0.2502 | 0.028 | 0.055 | 0.028 | 98.14 | |||
Stearic acid (SA) | 0.2500 | 0.015 | 0.028 | 0.013 | 100.79 | 102.05 | 4.60 |
0.2500 | 0.015 | 0.028 | 0.013 | 100.02 | |||
0.2499 | 0.015 | 0.029 | 0.013 | 107.76 | |||
0.2502 | 0.015 | 0.028 | 0.013 | 99.91 | |||
0.2499 | 0.015 | 0.028 | 0.013 | 96.22 | |||
0.2502 | 0.015 | 0.029 | 0.013 | 107.60 | |||
Oleic acid (OA) | 0.2500 | 0.087 | 0.174 | 0.085 | 101.79 | 98.82 | 2.22 |
0.2500 | 0.087 | 0.170 | 0.085 | 97.08 | |||
0.2499 | 0.087 | 0.169 | 0.085 | 95.94 | |||
0.2502 | 0.088 | 0.172 | 0.085 | 99.33 | |||
0.2499 | 0.087 | 0.173 | 0.085 | 100.65 | |||
0.2502 | 0.088 | 0.171 | 0.085 | 98.15 | |||
Linoleic acid (LA) | 0.2500 | 0.077 | 0.137 | 0.060 | 99.19 | 100.83 | 3.84 |
0.2500 | 0.077 | 0.136 | 0.060 | 97.53 | |||
0.2499 | 0.077 | 0.138 | 0.060 | 100.91 | |||
0.2502 | 0.078 | 0.140 | 0.060 | 104.06 | |||
0.2499 | 0.077 | 0.141 | 0.060 | 105.91 | |||
0.2502 | 0.078 | 0.136 | 0.060 | 97.40 |
Sample Number | PA (%) | SA (%) | OA (%) | LA (%) | Total Amount (%) |
---|---|---|---|---|---|
S1 | 0.27 | 0.08 | 1.01 | 0.65 | 2.01 |
S2 | 0.25 | 0.07 | 0.89 | 0.57 | 1.78 |
S3 | 0.23 | 0.07 | 0.86 | 0.56 | 1.72 |
S4 | 0.25 | 0.07 | 0.88 | 0.58 | 1.78 |
S5 | 0.23 | 0.07 | 0.84 | 0.55 | 1.69 |
S6 | 0.26 | 0.08 | 0.95 | 0.63 | 1.92 |
S7 | 0.26 | 0.07 | 0.92 | 0.60 | 1.85 |
S8 | 0.25 | 0.07 | 0.88 | 0.58 | 1.78 |
S9 | 0.22 | 0.07 | 0.82 | 0.55 | 1.66 |
S10 | 0.30 | 0.08 | 1.14 | 0.69 | 2.21 |
S11 | 0.22 | 0.07 | 0.83 | 0.54 | 1.66 |
S12 | 0.19 | 0.07 | 0.74 | 0.49 | 1.49 |
S13 | 0.22 | 0.07 | 0.80 | 0.54 | 1.63 |
S14 | 0.18 | 0.07 | 0.68 | 0.47 | 1.4 |
S15 | 0.22 | 0.07 | 0.81 | 0.52 | 1.62 |
S16 | 0.17 | 0.06 | 0.61 | 0.44 | 1.28 |
S17 | 0.21 | 0.07 | 0.74 | 0.53 | 1.55 |
S18 | 0.30 | 0.07 | 1.15 | 0.66 | 2.18 |
S19 | 0.24 | 0.07 | 0.91 | 0.59 | 1.81 |
S20 | 0.32 | 0.08 | 1.17 | 0.73 | 2.3 |
S21 | 0.23 | 0.07 | 0.79 | 0.54 | 1.63 |
S22 | 0.23 | 0.07 | 0.84 | 0.54 | 1.68 |
S23 | 0.21 | 0.07 | 0.75 | 0.51 | 1.54 |
S24 | 0.11 | 0.06 | 0.35 | 0.31 | 0.83 |
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Ai, Q.; Wang, H.; Xiao, C.; Yang, C.; Song, S.; Zhang, M.; Tang, J.; Lei, Y. Simultaneous Determination of Four Fatty Acids in Coix Seeds via Gas Chromatography. ChemEngineering 2025, 9, 98. https://doi.org/10.3390/chemengineering9050098
Ai Q, Wang H, Xiao C, Yang C, Song S, Zhang M, Tang J, Lei Y. Simultaneous Determination of Four Fatty Acids in Coix Seeds via Gas Chromatography. ChemEngineering. 2025; 9(5):98. https://doi.org/10.3390/chemengineering9050098
Chicago/Turabian StyleAi, Qiang, Hui Wang, Chenghong Xiao, Changgui Yang, Shanmin Song, Mingxiang Zhang, Jiandong Tang, and Yang Lei. 2025. "Simultaneous Determination of Four Fatty Acids in Coix Seeds via Gas Chromatography" ChemEngineering 9, no. 5: 98. https://doi.org/10.3390/chemengineering9050098
APA StyleAi, Q., Wang, H., Xiao, C., Yang, C., Song, S., Zhang, M., Tang, J., & Lei, Y. (2025). Simultaneous Determination of Four Fatty Acids in Coix Seeds via Gas Chromatography. ChemEngineering, 9(5), 98. https://doi.org/10.3390/chemengineering9050098