Abstract
Avermectins were illegally used and detected in aquaculture recently. In this study, a process, robustness, improvements, matrix effects, ease of use (PRiME) pass-through solid-phase extraction (SPE) was developed for the purification of avermectins in grass carp (Ctenopharyngodon idella) tissue. The eluate was directly analyzed by ultra-performance liquid chromatography (UPLC) and tandem mass spectrometry (MS/MS). The conditions were optimized by using 90% methanol (0.1% formic acid) as extracting solvent with volume of 3 mL. The MS/MS parameters were also tested for selecting the optimum precursor ions, such as [M+H]+ and [M+NH4]+. Afterwards, this methodology was validated in terms of linearity (0.9989–0.9997), limit of detection (LOD ≤ 1.10 μg kg−1), precision (RSD 1.88–4.85%), recovery (76.3–90.7%), etc., indicating its efficiency and robustness. Finally, five batches of grass carps (n = 6) from local markets were analyzed, and the results indicated the presence of abamectin in two fish samples originating from illegal use or cross contamination of drug. The PRiME technique can simplify the sample preparation procedure by avoiding the tedious steps, such as conditioning and washing. The successful application of the PRiME SPE and UPLC-MS/MS method indicated its superiority in detecting low levels of avermectins from the violation of regulation.
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References
Chen ZY, Ying S, Liu JH, Zhan PP, Zhao YG (2016) PRiME pass-through cleanup for the fast determination of aflatoxins in human serum by using LC-MS/MS. Anal Methods 8(7):1457–1462. https://doi.org/10.1039/c5ay03099d
Chen K, Wang J, Li S, Wang Y, Zhang Y, Shen Q (2018) High-throughput 96-well solid-phase extraction for preparation of tetracycline followed by liquid chromatography and mass spectrometry analysis. Electrophoresis 40(4):555–562. https://doi.org/10.1002/elps.201800473
Croubels S, De Baere S, Cherlet M, De Backer P (2002) Determination of ivermectin B1a in animal plasma by liquid chromatography combined with electrospray ionization mass spectrometry. J Mass Spectrom 37(8):840–847. https://doi.org/10.1002/jms.343
Cui Y, Shen N, Wang S, Mei L, Liu Z, Dang J, Tao Y (2017) Trace anti-inflammatory β-carboline alkaloid identified in Arenaria kansuensis by two-dimensional chromatography coupled with UniElut C18AEX based solid-phase extraction re-enrichment technology. J Chromatogr B 1068:282–288. https://doi.org/10.1016/j.jchromb.2017.10.058
Du P, Liu X, Gu X, Dong F, Xu J, Kong Z, Wu Y, Zhu Y, Li Y, Zheng Y (2013) Rapid residue analysis of pyriproxyfen, avermectins and diflubenzuron in mushrooms by ultra-performance liquid chromatography coupled with tandem mass spectrometry. Anal Methods 5(23):6741–6747. https://doi.org/10.1039/c3ay41074a
Ganguly S, Mahanty A, Mitra T, Mohanty S, Das BK, Mohanty BP (2018) Nutrigenomic studies on hilsa to evaluate flesh quality attributes and genes associated with fatty acid metabolism from the rivers Hooghly and Padma. Food Res Int 103:21–29. https://doi.org/10.1016/j.foodres.2017.10.017
García-Mayor MA, Gallego-Picó A, Garcinuño RM, Fernández-Hernando P, Durand-Alegría JS (2012) Matrix solid-phase dispersion method for the determination of macrolide antibiotics in sheep’s milk. Food Chem 134(1):553–558. https://doi.org/10.1016/j.foodchem.2012.02.120
He L, Pei Y, Jiang Y, Li Y, Liao L, Zhu Z, Wang Y (2015) Global gene expression patterns of grass carp following compensatory growth. BMC Genomics 16(1):184. https://doi.org/10.1186/s12864-015-1427-2
He SW, Zhao YG, Zhang Y, Jin MC, Zhu Y (2018) Hydrophilicity nano-titania coating modified magnetic graphene oxide for pass-through cleanup of fipronil and its metabolites in human blood. J Chromatog A 1553:16–24. https://doi.org/10.1016/j.chroma.2018.04.019
Hernando MD, Suarez-Barcena JM, Bueno MJM, Garcia-Reyes JF, Fernandez-Alba AR (2007) Fast separation liquid chromatography-tandem mass spectrometry for the confirmation and quantitative analysis of avermectin residues in food. J Chromatogr A 1155(1):62–73. https://doi.org/10.1016/j.chroma.2007.02.120
Hou X, Wu Y, Shen J, Wang L, Ding S (2007) Multi-residue analysis of avermectins in bovine liver and muscle by liquid chromatography-fluorescence detector. Chromatographia 65(1–2):77–80. https://doi.org/10.1365/s10337-006-0098-1
Huang T, Zhang W, Dai X, Li N, Huang L, Quan C, Li H, Yang Y (2016) High performance liquid chromatography-quantitative nuclear magnetic resonance (HPLC-qNMR) with a two-signal suppression method for purity assessment of avermectin B1a. Anal Methods 8(22):4482–4486. https://doi.org/10.1039/c6ay00570e
Krogh KA, Björklund E, Loeffler D, Fink G, Halling-Sørensen B, Ternes TA (2008) Development of an analytical method to determine avermectins in water, sediments and soils using liquid chromatography–tandem mass spectrometry. J Chromatogr A 1211(1–2):60–69. https://doi.org/10.1016/j.chroma.2008.09.081
Ma JB, Zhao LM, Rui QH, Liao YF, Chen YM, Xu J, Zhu Y, Zhao YG (2017) Application of carbon nanosorbent for PRiME pass-through cleanup of 10 selected local anesthetic drugs in human plasma samples. Anal Chim Acta 960:72–80. https://doi.org/10.1016/j.aca.2017.01.033
Monsalve S, Ferreira F, Garcia R (2017) The connection between animal abuse and interpersonal violence: a review from the veterinary perspective. Res Vet Sci 114:18–26. https://doi.org/10.1016/j.rvsc.2017.02.025
Moschou IC, Dasenaki ME, Thomaidis NS (2019) Ionization study and simultaneous determination of avermectins and milbemycines in fish tissue by LC-ESI-MS/MS. J Chromatogr B 1104:134–140. https://doi.org/10.1016/j.jchromb.2018.11.017
Ozdemir N, Kahraman T (2016) Rapid confirmatory analysis of avermectin residues in milk by liquid chromatography tandem mass spectrometry. J Food Drug Anal 24(1):90–94. https://doi.org/10.1016/j.jfda.2015.07.004
Rezaee M, Mashayekhi HA, Saleh A, Abdollahzadeh Y, Naeeni MH, Fattahi N (2013) Determination of abamectin in citrus fruits using SPE combined with dispersive liquid-liquid microextraction and HPLC-UV detection. J Sep Sci 36(16):2629–2634. https://doi.org/10.1002/jssc.201300356
Rübensam G, Barreto F, Hoff RB, Pizzolato TM (2013) Determination of avermectin and milbemycin residues in bovine muscle by liquid chromatography-tandem mass spectrometry and fluorescence detection using solvent extraction and low temperature cleanup. Food Control 29(1):55–60. https://doi.org/10.1016/j.foodcont.2012.05.075
Rúbies A, Antkowiak S, Granados M, Companyó R, Centrich F (2015) Determination of avermectins: a QuEChERS approach to the analysis of food samples. Food Chem 181:57–63. https://doi.org/10.1016/j.foodchem.2015.02.067
Shen Q, Dai Z, Lu Y (2010) Rapid determination of caffeoylquinic acid derivatives in Cynara scolymus L. by ultra-fast liquid chromatography/tandem mass spectrometry based on a fused core C18 column. J Sep Sci 33(20):3152–3158. https://doi.org/10.1002/jssc.201000397
Shen Q, Dong W, Wang Y, Gong L, Dai Z, Cheung HY (2013a) Pipette tip solid-phase extraction and ultra-performance liquid chromatography/mass spectrometry based rapid analysis of picrosides from Picrorhiza scrophulariiflora. J Pharm Biomed Anal 80:136–140. https://doi.org/10.1016/j.jpba.2013.03.002
Shen Q, Dong W, Wang Y, Zhu Z, Gong L, Dai Z, Zhang H, Cheung HY (2013b) Automated online solid-phase extraction of albendazole and its metabolites in Chinese mitten crabs followed by stable isotope dilution UPLC-MS/MS analysis. Eur Food Res Technol 236(5):919–929. https://doi.org/10.1007/s00217-013-1952-7
Shen Q, Gong L, Baibado JT, Dong W, Wang Y, Dai Z, Cheung HY (2013c) Graphene based pipette tip solid phase extraction of marine toxins in shellfish muscle followed by UPLC-MS/MS analysis. Talanta 116:770–775. https://doi.org/10.1016/j.talanta.2013.07.042
Tao Y, Yu G, Chen D, Pan Y, Liu Z, Wei H, Peng D, Huang L, Wang Y, Yuan Z (2012) Determination of 17 macrolide antibiotics and avermectins residues in meat with accelerated solvent extraction by liquid chromatography-tandem mass spectrometry. J Chromatogr B 897:64–71. https://doi.org/10.1016/j.jchromb.2012.04.011
Thompson TS, Noot DK, Forrest F, van Den Heever JP, Kendall J, Keenliside J (2009) Large volume injection for the direct analysis of ionophores and avermectins in surface water by liquid chromatography-electrospray ionization tandem mass spectrometry. Anal Chim Acta 633(1):127–135. https://doi.org/10.1016/j.aca.2008.11.024
Wang H, Wang Z, Liu S, Liu Z (2009) Rapid method for multi-residue determination of avermectins in bovine liver using high-performance liquid chromatography with fluorescence detection. Bull Environ Contam Toxicol 82(4):395–398. https://doi.org/10.1007/s00128-009-9638-3
Wang Y, Lu Y, Zhang Y, Ning Z, Li Y, Zhao Q, Lu H, Huang R, Xia X, Feng Q, Liang X, Liu K, Zhang L, Lu T, Huang T, Fan D, Weng Q, Zhu C, Lu Y, Li W, Wen Z, Zhou C, Tian Q, Kang X, Shi M, Zhang W, Jang S, du F, He S, Liao L, Li Y, Gui B, He H, Ning Z, Yang C, He L, Luo L, Yang R, Luo Q, Liu X, Li S, Huang W, Xiao L, Lin H, Han B, Zhu Z (2015) The draft genome of the grass carp (Ctenopharyngodon idellus) provides insights into its evolution and vegetarian adaptation. Nat Genet 47(6):625–631. https://doi.org/10.1038/ng.3280
Yu X, Yang H (2017) Pyrethroid residue determination in organic and conventional vegetables using liquid-solid extraction coupled with magnetic solid phase extraction based on polystyrene-coated magnetic nanoparticles. Food Chem 217:303–310. https://doi.org/10.1016/j.foodchem.2016.08.115
Yu X, Li Y, Ng M, Yang H, Wang S (2018) Comparative study of pyrethroids residue in fruit peels and fleshes using polystyrene-coated magnetic nanoparticles based clean-up techniques. Food Control 85:300–307. https://doi.org/10.1016/j.foodcont.2017.10.016
Zhang M, Chen K, Hu Z, Shen Q, Wang H (2018a) PRiME pass-through purification of lignans in Silybum marianum and UPLC-MS/MS analysis. J Chromatogr B 1093:128-133:128–133. https://doi.org/10.1016/j.jchromb.2018.07.003
Zhang Y, Zhao YG, Cheng HL, Muhammad N, Chen WS, Zeng XQ, Zhu Y (2018b) Fast determination of fipronil and its metabolites in seafood using PRiME pass-through cleanup followed by isotope dilution UHPLC-MS/MS. Anal Methods 10(15):1673–1679. https://doi.org/10.1039/c8ay00445e
Funding
This study was funded by the Quality & Safety of Aquatic Products Technical Support Team (QS2018001), Zhejiang Province Public Welfare Technology Application Research Project (LGF19H180013), and Qianjiang Talent Program of Zhejiang Province.
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Yiqi Zhang declares that he has no conflict of interest. Xina Yu declares that she has no conflict of interest. Linqiu Li declares that she has no conflict of interest. Yi Chen declares that he has no conflict of interest. Jie Wang declares that he has no conflict of interest. Qing Shen declares that he has no conflict of interest.
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Zhang, Y., Yu, X., Li, L. et al. Development of a PRiME Cleanup Procedure for the Purification of Avermectins in Grass Carps and Liquid Chromatography-Tandem Mass Spectrometry Analysis. Food Anal. Methods 12, 1905–1913 (2019). https://doi.org/10.1007/s12161-019-01542-3
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DOI: https://doi.org/10.1007/s12161-019-01542-3