A modified QuEChERS protocol with a nitrogen-doped graphitized carbon derived from dicyandiamide sludge as a cleanup sorbent has been developed to determine 20 organochlorine pesticides in tomatoes using gas chromatography coupled to a triple-quadrupole mass analyzer. Compared with traditional QuEChERS adsorbents, N-doped graphitized carbon exhibited higher recoveries toward the target pesticides in tomatoes. And the modified protocol exhibited the advantages of environmental-friendly and low-cost. The use of dicyandiamide sludge to produce NGB as an adsorbent for QuEChERS opened up a new field for the comprehensive utilization of dicyandiamide waste. Under the optimum conditions, the modified method provided excellent linearity with correlation coefficient higher than 0.9980 and low limits of detection ranging from 0.001 to 0.1 μg/kg. The mean recoveries of the majority of pesticides in tomatoes ranged from 71.2 to 95.3% with relative standard deviation lower than 20%. Thus, the proposed protocol could be considered a good alternative for traditional QuEChERS method for pesticide analysis in agricultural vegetables.
This is a preview of subscription content, log in to check access.
Buy single article
Instant access to the full article PDF.
Price includes VAT for USA
Subscribe to journal
Immediate online access to all issues from 2019. Subscription will auto renew annually.
This is the net price. Taxes to be calculated in checkout.
Cheng J, Hu Z, Lv K, Wu X, Li Q, Li Y, Li X, Sun J (2018) Drastic promoting the visible photoreactivity of layered carbon nitride by polymerization of dicyandiamide at high pressure. Appl Catal B Environ 232:330–339
Dong H, Xian Y, Xiao K, Wu Y, Zhu L, He J (2019) Development and comparison of single-step solid phase extraction and QuEChERS clean-up for the analysis of 7 mycotoxins in fruits and vegetables during storage by UHPLC-MS/MS. Food Chem 274:471–479
European Union (2008) Pesticide EU-MRLs, Regulation (EC) No. 839/2008. http://ec.europa.eu/food/plant/pesticides/eu-pesticides-database/public/?event = pesticide.residue.selection&language = EN
Guo J, Tong M, Tang J, Bian H, Wan X, He L, Hou R (2019) Analysis of multiple pesticide residues in polyphenol-rich agricultural products by UPLC-MS/MS using a modified QuEChERS extraction and dilution method. Food Chem 274:452–459
Han XF, Chen J, Shi YP (2018) N-doped carbon nanotubes-reinforced hollow fiber solid-phase microextraction coupled with high performance liquid chromatography for the determination of phytohormones in tomatoes. Talanta 185:132–140
Huang Y, Shi T, Luo X, Xiong H, Min F, Chen Y, Nie S, Xie M (2019) Determination of multi-pesticide residues in green tea with a modified QuEChERS protocol coupled to HPLC-MS/MS. Food Chem 275:255–264
Jiang HL, Lin YL, Li N, Wang ZW, Liu M, Zhao RS, Lin JM (2018) Application of magnetic N-doped carbon nanotubes in solid-phase extraction of trace bisphenols from fruit juices. Food Chem 269:413–418
Kang J, Wu MX (2018) Utilization status and development prospect of dicyandiamide waste residue resources. Guangzhou Chem Ind 46:121–123
Li YF, Qiao LQ, Li FW, Ding Y, Yang ZJ, Wang ML (2014) Determination of multiple pesticides in fruits and vegetables using a modified quick, easy, cheap, effective, rugged and safe method with magnetic nanoparticles and gas chromatography tandem mass spectrometry. J Chromatogr A 1361:77–87
Li M, Jiao C, Yang X, Wang C, Wu Q, Wang Z (2017) Magnetic N-doped mesoporous carbon as an adsorbent for the magnetic solid-phase extraction of phthalate esters from soft drinks. J Sep Sci 40:1637–1643
Li P, Duan Y, Ge H, Zhang Y, Wu X (2018) Multiresidue analysis of 113 pesticides in different maturity levels of mangoes using an optimized QuEChERS method with GC-MS/MS and UHPLC-MS/MS. Food Anal Methods 11:2742–2757
Lu Y, Cheng Z, Liu C, Cao X (2016) Determination of sulfonamides in fish using a modified QuEChERS extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry. Food Anal Methods 9:1857–1866
Nsabimana A, Lai J, Li S, HUi P, Liu Z, Xu G (2017) Surfactant-free synthesis of three-dimensional nitrogen-doped hierarchically porous carbon and its application as an electrode modification material for simultaneous sensing of ascorbic acid, dopamine and uric acid. Analyst 142:478–484
People’s Republic of China (2016) National food safety standard-Maximum residue limits for pesticides in food. GB: 2763-2016. http://www.doc88.com/p-3458467515607.html
Salamzadeh J, Shakoori A, Moradi V (2018) Occurrence of multiclass pesticide residues in tomato samples collected from different markets of Iran. J Environ Health Sci Eng 16:55–63
Xie YL, Zhao ZD, Zhang XL, Tang LL, Zhang Y, Zhang CH (2017) Simultaneous analysis of herbicide metribuzin and its transformation products in tomato using QuEChERS-based gas chromatography coupled to a triple quadrupole mass analyzer. Microchem J 133:468–473
Yang YJ (2016) Study on the process of preparation of active calcium oxide slag derived from dicyandiamide. Dissertation, Ningxia University
Yang L, Liu X, Liu Z, Wang C, Liu G, Li Q, Feng X (2018) Enhanced photocatalytic activity of g-C3N4 2D nanosheets through thermal exfoliation using dicyandiamide as precursor. Ceram Int 44:20613–20619
Zawiyah S, Man YBC, Nazimah SAH, Chin CK, Tsukamoto I, Hamanyza AH, Norhaizan I (2007) Determination of organochlorine and pyrethroid pesticides in fruit and vegetables using SAX/PSA clean-up column. Food Chem 102:98–103
Zhan XP, Ma L, Huang L, Chen J, Zhao L (2017) The optimization and establishment of QuEChERS-UPLC–MS/MS method for simultaneously detecting various kinds of pesticides residues in fruits and vegetables. J Chromatogr B 1060:281–290
Zheng HB, Zhao Q, Mo JZ, Huang YQ, Luo YB, Yu QW, Feng YQ (2013) Quick, easy, cheap, effective, rugged and safe method with magnetic graphitized carbon black and primary secondary amine as adsorbent and its application in pesticide residue analysis. J Chromatogr A 1300: 127–133
The authors also acknowledge the contributions of Maiqi Chen to our works of partial data analysis and processing.
This study was financially supported by Zhejiang Province Public Welfare Technology Application Research Project (2017C37008, 2017C33014).
Conflict of Interest
Xuemin Ye declares that she has no conflict of interest. Hua Shao declares that he has no conflict of interest. Ting Zhou declares that she has no conflict of interest. Jiahui Xu declares that he has no conflict of interest. Xiaoji Cao declares that she has no conflict of interest. Weimin Mo declares that he has no conflict of interest.
This article does not contain any studies with human participants or animals performed by any of the authors.
Informed consent is not applicable for this study.
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
About this article
Cite this article
Ye, X., Shao, H., Zhou, T. et al. Analysis of Organochlorine Pesticides in Tomatoes Using a Modified QuEChERS Method Based on N-Doped Graphitized Carbon Coupled with GC-MS/MS. Food Anal. Methods 13, 823–832 (2020). https://doi.org/10.1007/s12161-019-01674-6
- N-doped graphitized carbon
- Organochlorine pesticides