Skip to main content
SpringerLink
Log in

Determination of Three Carotenoids in Microalgae by Matrix Solid-Phase Dispersion Extraction and High-Performance Liquid Chromatography

  • Original
  • Published:
Chromatographia Aims and scope Submit manuscript

Abstract

A HPLC method based on matrix solid-phase dispersion (MSPD) was developed for simultaneous determination of fucoxanthin, lutein and astaxanthin in different microalgae. First, the powder of microalgae was blended with C8 adsorbent. Then the SPE column made from the microalgal matrix/sorbent (1:2) was eluted with 4 mL methanol (containing 0.1% BHT). The eluent was analyzed by HPLC. A C8 column and acetonitrile (ACN)/H2O as the mobile phase were used. The coefficient (R2) of each calibration curve was higher than 0.998. Limits of detection (LODs) and limits of quantification (LOQs) for each carotenoid were 0.30 µg g−1 and 1.00 µg g−1, respectively. The recovery at three concentration levels ranged from 69.1 to 106.5%, and the RSDs were lower than 5%. As a new sample preparation method for microalgal analysis, the MSPD procedure was optimized, validated and compared with conventional methods including ultrasonic and ice-bath extraction. The MSPD–HPLC method was accurate and reproducible. It was suitable for the quantitative determination of carotenoids in microalgae.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8

Similar content being viewed by others

Abbreviations

BHT:

Butylated hydroxytoluene

MTBE:

Methyl tert-butyl ether

PTFE:

Polytetrafluoroethylene

References

  1. Ahmed F, Fanning K, Netzel M, Turner W, Li Y, Schenk PM (2014) Profiling of carotenoids and antioxidant capacity of microalgae from subtropical coastal and brackish waters. Food Chem 165:300–306. https://doi.org/10.1016/j.foodchem.2014.05.107

    Article  CAS  PubMed  Google Scholar 

  2. Chan M-C, Ho S-H, Lee D-J, Chen C-Y, Huang C-C, Chang J-S (2013) Characterization, extraction and purification of lutein produced by an indigenous microalga Scenedesmus obliquus CNW-N. Biochem Eng J 78:24–31. https://doi.org/10.1016/j.bej.2012.11.017

    Article  CAS  Google Scholar 

  3. Yuan JP, Chen F (2000) Purification of trans-astaxanthin from a high-yielding astaxanthin ester-producing strain of the microalga Haematococcus pluvialis. Food Chem 68(4):443–448. https://doi.org/10.1016/s0308-8146(99)00219-8

    Article  CAS  Google Scholar 

  4. Xia S, Wang K, Wan L, Li A, Hu Q, Zhang C (2013) Production, characterization, and antioxidant activity of fucoxanthin from the marine diatom Odontella aurita. Mar Drugs 11(7):2667–2681. https://doi.org/10.3390/md11072667

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  5. Campenni L, Nobre BP, Santos CA, Oliveira AC, Aires-Barros MR, Palavra AMF, Gouveia L (2013) Carotenoid and lipid production by the autotrophic microalga Chlorella protothecoides under nutritional, salinity, and luminosity stress conditions. Appl Microbiol Biotechnol 97(3):1383–1393. https://doi.org/10.1007/s00253-012-4570-6

    Article  CAS  PubMed  Google Scholar 

  6. Esquivel-Hernandez DA, Ibarra-Garza IP, Rodriguez-Rodriguez J, Cuellar-Bermudez SP, Rostro-Alanis MdJ, Aleman-Nava GS, Garcia-Perez JS, Parra-Saldivar R (2017) Green extraction technologies for high-value metabolites from algae: a review. Biofuels Bioprod Biorefining-Biofpr 11(1):215–231. https://doi.org/10.1002/bbb.1735

    Article  CAS  Google Scholar 

  7. Billakanti JM, Catchpole OJ, Fenton TA, Mitchell KA, MacKenzie AD (2013) Enzyme-assisted extraction of fucoxanthin and lipids containing polyunsaturated fatty acids from Undaria pinnatifida using dimethyl ether and ethanol. Process Biochem 48(12):1999–2008. https://doi.org/10.1016/j.procbio.2013.09.015

    Article  CAS  Google Scholar 

  8. Nobre B, Marcelo F, Passos R, Beirao L, Palavra A, Gouveia L, Mendes R (2006) Supercritical carbon dioxide extraction of astaxanthin and other carotenoids from the microalga Haematococcus pluvialis. Eur Food Res Technol 223(6):787–790. https://doi.org/10.1007/s00217-006-0270-8

    Article  CAS  Google Scholar 

  9. Wianowska D, Dawidowicz AL (2016) Can matrix solid phase dispersion (MSPD) be more simplified? Application of solventless MSPD sample preparation method for GC-MS and GC-FID analysis of plant essential oil components. Talanta 151:179–182. https://doi.org/10.1016/j.talanta.2016.01.019

    Article  CAS  PubMed  Google Scholar 

  10. Huang Z, Pan X-D, Huang B-f, Xu J-J, Wang M-L, Ren Y-P (2016) Determination of 15 beta-lactam antibiotics in pork muscle by matrix solid-phase dispersion extraction (MSPD) and ultra-high pressure liquid chromatography tandem mass spectrometry. Food Control 66:145–150. https://doi.org/10.1016/j.foodcont.2016.01.037

    Article  CAS  Google Scholar 

  11. Tao Y, Zhu F, Chen D, Wei H, Pan Y, Wang X, Liu Z, Huang L, Wang Y, Yuan Z (2014) Evaluation of matrix solid-phase dispersion (MSPD) extraction for multi-fenicols determination in shrimp and fish by liquid chromatography-electrospray ionisation tandem mass spectrometry. Food Chem 150:500–506. https://doi.org/10.1016/j.foodchem.2013.11.013

    Article  CAS  PubMed  Google Scholar 

  12. Cao Y, Tang H, Chen D, Li L (2015) A novel method based on MSPD for simultaneous determination of 16 pesticide residues in tea by LC-MS/MS. J Chromatogr B-Anal Technol Biomed Life Sci 998:72–79. https://doi.org/10.1016/j.jchromb.2015.06.013

    Article  CAS  Google Scholar 

  13. Dawidowicz AL, Wianowska D (2009) Application of the MSPD technique for the HPLC analysis of rutin in Sambucus nigra L.: the linear correlation of the matrix solid-phase dispersion process. J Chromatogr Sci 47(10):914–918. https://doi.org/10.1093/chromsci/47.10.914

    Article  CAS  PubMed  Google Scholar 

  14. Dias Soares CM, Fernandes JO (2009) MSPD method to determine acrylamide in food. Food Anal Methods 2(3):197–203. https://doi.org/10.1007/s12161-008-9060-1

    Article  Google Scholar 

  15. Chen J-h, Zhou G-m, Qin H-y, Gao Y, Peng G-l (2015) Organic solvent-free matrix solid phase dispersion (MSPD) for determination of synthetic colorants in chilli powder by high-performance liquid chromatography (HPLC-UV). Anal Methods 7(16):6537–6544. https://doi.org/10.1039/c5ay01105a

    Article  CAS  Google Scholar 

  16. Dawidowicz AL, Wianowska D, Rado E (2011) Matrix solid-phase dispersion with sand in chromatographic analysis of essential oils in herbs. Phytochem Anal 22(1):51–58. https://doi.org/10.1002/pca.1250

    Article  CAS  PubMed  Google Scholar 

  17. Xiao HB, Krucker M, Albert K, Liang XM (2004) Determination and identification of isoflavonoids in Radix astragali by matrix solid-phase dispersion extraction and high-performance liquid chromatography with photodiode array and mass spectrometric detection. J Chromatogr A 1032(1–2):117–124. https://doi.org/10.1016/j.chroma.2003.09.032

    Article  CAS  PubMed  Google Scholar 

  18. Ceron-Garcia MC, Gonzalez-Lopez CV, Camacho-Rodriguez J, Lopez-Rosales L, Garcia-Camacho F, Molina-Grima E (2018) Maximizing carotenoid extraction from microalgae used as food additives and determined by liquid chromatography (HPLC). Food Chem 257:316–324. https://doi.org/10.1016/j.foodchem.2018.02.154

    Article  CAS  PubMed  Google Scholar 

  19. Wald JP, Nohr D, Biesalski HK (2018) Rapid and easy carotenoid quantification in Ghanaian starchy staples using RP-HPLC-PDA. J Food Compos Anal 67:119–127. https://doi.org/10.1016/j.jfca.2018.01.006

    Article  CAS  Google Scholar 

  20. Aluc Y, Kankilic GB, Tuzun I (2018) Determination of carotenoids in two algae species from the saline water of Kapulukaya reservoir by HPLC. J Liq Chromatogr Relat Technol 41(2):93–100. https://doi.org/10.1080/10826076.2017.1418376

    Article  CAS  Google Scholar 

  21. Zeb A (2017) A simple, sensitive HPLC-DAD method for simultaneous determination of carotenoids, chlorophylls and alpha-tocopherol in leafy vegetables. J Food Meas Char 11(3):979–986. https://doi.org/10.1007/s11694-017-9472-y

    Article  Google Scholar 

  22. Strati IF, Sinanoglou VJ, Kora L, Miniadis-Meimaroglou S, Oreopoulou V (2012) Carotenoids from foods of plant, animal and marine origin: an efficient HPLC-DAD separation method. Foods (Basel, Switzerland) 1(1):52–65. https://doi.org/10.3390/foods1010052

    Article  CAS  Google Scholar 

  23. Glaser T, Lienau A, Zeeb D, Krucker M, Dachtler M, Albert K (2003) Qualitative and quantitative determination of carotenoid stereoisomers in a variety of spinach samples by use of MSPD before HPLC-UV, HPLC-APCI-MS, and HPLC-NMR on-line coupling. Chromatographia 57:S19–S25. https://doi.org/10.1007/bf02492079

    Article  Google Scholar 

  24. Melendez-Martinez AJ, Vicario IM, Heredia FJ (2003) A routine high-performance liquid chromatography method for carotenoid determination in ultrafrozen orange juices. J Agric Food Chem 51(15):4219–4224. https://doi.org/10.1021/jf0342977

    Article  CAS  PubMed  Google Scholar 

  25. Akhtar MH, Bryan M (2008) Extraction and quantification of major carotenoids in processed foods and supplements by liquid chromatography. Food Chem 111(1):255–261. https://doi.org/10.1016/j.foodchem.2008.03.071

    Article  CAS  Google Scholar 

Download references

Funding

This study was funded by Project of National Natural Science Foundation of China (No. 21505131), Natural Science Foundation of Liaoning Province (2015021015) and the Creative Research Group Project of NSFC (21321064).

Author information

Authors and Affiliations

  1. CAS Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian, 116023, China

    Gaowa Jin, Song Xue, Yingying Meng, Jingyu Yan, Fan Yang, Zhimou Guo & Xinmiao Liang

  2. Shandong Institute of Food and Drug Control, Jinan, 250101, China

    Yanming Liu & Jianhua Zhu

  3. Co-innovation Center of Neuroregeneration, Nantong University, Nantong, 226019, China

    Zhimou Guo & Xinmiao Liang

Authors
  1. Gaowa Jin
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Yanming Liu
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Song Xue
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Yingying Meng
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Jingyu Yan
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Fan Yang
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Zhimou Guo
    View author publications

    You can also search for this author in PubMed Google Scholar

  8. Jianhua Zhu
    View author publications

    You can also search for this author in PubMed Google Scholar

  9. Xinmiao Liang
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding authors

Correspondence to Zhimou Guo or Xinmiao Liang.

Ethics declarations

Conflict of interest

The authors declare that they have no conflict of interest.

Ethical approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Jin, G., Liu, Y., Xue, S. et al. Determination of Three Carotenoids in Microalgae by Matrix Solid-Phase Dispersion Extraction and High-Performance Liquid Chromatography. Chromatographia 82, 1593–1601 (2019). https://doi.org/10.1007/s10337-019-03795-w

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10337-019-03795-w

Keywords

Search

Navigation