Skip to main page content
U.S. flag

An official website of the United States government

Dot gov

The .gov means it’s official.
Federal government websites often end in .gov or .mil. Before sharing sensitive information, make sure you’re on a federal government site.

Https

The site is secure.
The https:// ensures that you are connecting to the official website and that any information you provide is encrypted and transmitted securely.

Access keys NCBI Homepage MyNCBI Homepage Main Content Main Navigation
. 2023 Jun 16;11(6):537.
doi: 10.3390/toxics11060537.

Simultaneous Analysis of 53 Pesticides in Safflower (Carthamus tinctorius L.) by Using LC-MS/MS Coupled with a Modified QuEChERS Technique

Wei Song  1   2 , Chuanyi Peng  2   3 , Yuxin Liu  1   2 , Fang Han  1   2 , Haitao Zhu  1   2 , Dianbing Zhou  1   2 , Yu Wang  1   2 , Lijun Chen  1   2 , Xiaodi Meng  1   2 , Ruyan Hou  2   3
Affiliations

Simultaneous Analysis of 53 Pesticides in Safflower (Carthamus tinctorius L.) by Using LC-MS/MS Coupled with a Modified QuEChERS Technique

Wei Song et al. Toxics. .

Abstract

Objective: An optimized quick, easy, cheap, effective, rugged, and safe (QuEChERS) technique was investigated and compared with the conventional QuEChERS technique for the simultaneous analysis of fifty-three pesticide residues in safflower using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS).

Method: Graphitic carbon nitride (g-C3N4) consisting of a major amount of carbon and nitrogen with a large surface area was used as a QuEChERS adsorbent instead of graphitized carbon black (GCB) for safflower extraction purification. Validation experiments were performed using spiked pesticide samples, and real samples were analyzed.

Results: The linearity of the modified QuEChERS technique was evaluated with high coefficients of determination (R-2) being higher than 0.99. The limits of detection were <10 μg/kg. The spiked recoveries ranged from 70.4% to 97.6% with a relative standard deviation of less than 10.0%. The fifty-three pesticides exhibited negligible matrix effects (<20%). Thiamethoxam, acetamiprid, metolachlor, and difenoconazole were detected in real samples using an established method.

Conclusion: This work provides a new g-C3N4-based modified QuEChERS technique for multi-pesticide residue analysis in complex food matrices.

Keywords: g-C3N4; liquid chromatography–tandem mass spectrometry; modified QuEChERS; pesticide residues; safflower.

PubMed Disclaimer

Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
X-ray diffraction pattern (a) and Fourier-transform infrared spectra (b) of g-C3N4.
Figure 2
Figure 2
High-resolution transmission electron microscope images of (a) g-C3N4 (100 nm), (b) g-C3N4 (500 nm), (c) mapping of g-C3N4, and (d) EDS of g-C3N4.
Figure 2
Figure 2
High-resolution transmission electron microscope images of (a) g-C3N4 (100 nm), (b) g-C3N4 (500 nm), (c) mapping of g-C3N4, and (d) EDS of g-C3N4.
Figure 3
Figure 3
Characteristic ion extraction chromatogram of 53 pesticides.
Figure 4
Figure 4
Purification effect of g-C3N4. (a) Original safflower extraction, (b) safflower extraction after adsorption, (c) original g-C3N4 powder, and (d) g-C3N4 powder after adsorption.
Figure 5
Figure 5
Influence of different QuEChERS techniques on the recoveries of 53 pesticides in safflower.
See this image and copyright information in PMC

References

    1. Kalyabina V.P., Esimbekova E.N., Kopylova K.V., Kratasyuk V.A. Pesticides: Formulants, distribution pathways and effects on human health—A review. Toxicol. Rep. 2021;8:1179–1192. doi: 10.1016/j.toxrep.2021.06.004. - DOI - PMC - PubMed
    1. Reeves W., McGuire M.K., Stokes M., Vicini J.L. Assessing the Safety of Pesticides in Food: How Current Regulations Protect Human Health. Adv. Nutr. 2019;10:80–88. doi: 10.1093/advances/nmy061. - DOI - PMC - PubMed
    1. Attia H., Harrathi J., Alamer K.H., Alsalmi F.A., Magne C., Khalil M. Effects of NaCl on antioxidant, antifungal, and antibacterial activities in safflower essential oils. Plants. 2021;10:2809. doi: 10.3390/plants10122809. - DOI - PMC - PubMed
    1. Alaiye A., Kaya E., Pınarbaşlı M.Ö., Harmancı N., Yıldırım C., Dönmez D.B., Cingi C. An experimental comparison of the analgesic and anti-inflammatory effects of safflower oil, benzydamine HCl, and naproxen sodium. J. Med. Food. 2020;23:862–869. doi: 10.1089/jmf.2019.0157. - DOI - PubMed
    1. Park Y.G., Cho J.H., Choi J., Ju E.M., Adam G.O., Hwang D. Immunomodulatory effects of Curcuma longa L. and Carthamus tinctorius L. on RAW 264.7 macrophages and cyclophosphamide-induced immunosuppression C57BL/6 mouse models. J. Funct. Foods. 2022;91:105000. doi: 10.1016/j.jff.2022.105000. - DOI

LinkOut - more resources