注射器内分散固相萃取-超高效液相色谱-串联质谱法快速测定茶叶中24种农药残留

doi:10.13305/j.cnki.jts.20210804.001

Abstract

Abstract: Based on the characteristics of tea matrix, a rapid pretreatment technology of in-syringe dispersive solid phase extraction (dSPE) was developed, and an analytical method based on ultra high performance liquid chromatography-tandem mass spectrometry was established for the detection of 24 pesticide residues in tea. Tea samples were extracted using acetonitrile, salted-out with MgSO₄, purified with primary secondary amine and graphitized carbon black as dispersive adsorbents in designed syringe devices, and detected by UPLC-MS/MS. Recoveries of 24 pesticides in black and green teas were 61.7%-98.8% at three spiked levels (0.01βmg·kg^-1, 0.05βmg·kg^-1 and 0.5βmg·kg^-1), which indicated high accuracy with the relative standard deviations of 0.4%-5.5%. The calibration curves of 24 pesticides in black and green teas showed good linearity with correlation coefficients (R²) higher than 0.995. The limits of detection (LOD) and the limits of quantitation (LOQ) were 0.05-5.36βμg·kg^-1 and 0.18-17.86βμg·kg^-1, respectively, which show high sensitivity of this method. Being simple, fast, less instrument required and time-saving, this method is suitable for quantification of multiple pesticide residues in tea.

Key words: tea, ultra high performance liquid chromatography-tandem mass spectrometry, pesticide residues, in-syringe dispersive solid phase extraction

CLC Number:

MA Jiali, WANG Chen, CHEN Hongping, CHAI Yunfeng, ZHU Li, LIU Xin. Rapid Determination of 24 Pesticide Residues in Tea by in-Syringe Dispersive Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Journal of Tea Science, 2021, 41(5): 717-730.

References

[1] 张菲. 我国茶叶出口结构与竞争力分析——基于不同类别和包装规格茶叶的探讨[J]. 中国茶叶, 2018, 40(9): 13-18.
Zhang F.Analysis of export structure and competitiveness for Chinese tea: discussion based on different categories and packaging specifications of tea[J]. China Tea, 2018, 40(9): 13-18.
[2] 陈思敏, 林腾奕, 李星星, 等. QuEChERS结合液相色谱-串联质谱法检测茶叶中34种农药残留[J]. 食品安全质量检测学报, 2020, 11(2): 507-515.
Chen S M, Lin T Y, Li X X, et al.Determination of 34 kinds of pesticide residues in tea by QuEChERS combined with liquid chromatography tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2020, 11(2): 507-515.
[3] 余璐, 宋伟, 吕亚宁, 等. 超高效液相色谱-四极杆-飞行时间质谱法快速筛查茶叶中的204种农药残留[J]. 色谱, 2015, 33(6): 597-612.
Yu L, Song W, Lü Y N, et al.Rapid determination of 204 pesticide residues in tea by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry[J]. Chinese Journal of Chromatography, 2015, 33(6): 597-612.
[4] 蒋迎, 郑平, 鲁成银. 基于基质固相分散萃取的茶叶中拟除虫菊酯多农残气相色谱测定[J]. 茶叶, 2007, 33(3): 147-149.
Jiang Y, Zheng P, Lu C Y.Multiresidue determination of pyrethroid pesticides in teas by matrix solid-phase disperse and gas chromatography[J]. Journal of Tea, 2007, 33(3): 147-149.
[5] Deng X J, Guo Q J, Chen X P, et al.Rapid and effective sample clean-up based on magnetic multiwalled carbon nanotubes for the determination of pesticide residues in tea by gas chromatography-mass spectrometry[J]. Food Chemistry, 2014, 145(7): 853-858.
[6] 王孝辉, 宛晓春, 侯如燕. 茶叶中吡虫啉农药残留的液相色谱检测方法[J]. 茶叶科学, 2012, 32(3): 203-209.
Wang X H, Wan X C, Hou R Y.A method for determination of imidacloprid residue in tea with UPLC-UV[J]. Journal of Tea Science, 2012, 32(3): 203-209.
[7] Antoni D R, Diana C, Jordi E, et al.A fast and reliable ultrahigh-performance liquid chromatography method to assess the fate of chlorophylls in teas and processed vegetable foodstuff[J]. Journal of Chromatography A, 2018, 1568: 69-79.
[8] 陈昌梅, 林明霞, 兰元. SPE-GC-MS/MS法测定茶叶中的76种农药残留[J]. 中国茶叶, 2020, 42(12): 52-61.
Chen C M, Lin M X, Lan Y.SPE-GC-MS/MS method for the determination of 76 pesticide residues in tea sample[J]. China Tea, 2020, 42(12): 52-61.
[9] 王瑾, 陆小磊, 徐建峰, 等. 固相萃取-气质联用法测定吡虫啉在茶叶中残留量[J]. 中国茶叶加工, 2011(4): 24-26.
Wang J, Lu X L, Xu J F, et al.Determination of imidacloprid residue in tea by SPE and GC-MS[J]. China Tea Process, 2011(4): 24-26.
[10] Cajka T, Sandy C, Bachanova V, et al.Streamlining sample preparation and gas chromatography-tandem mass spectrometry analysis of multiple pesticide residues in tea[J]. Analytica Chimica Acta, 2012, 743: 51-60.
[11] 张艳侠, 张婷, 薛霞, 等. QuEChERS/超高效液相色谱-串联质谱法测定茶叶中17种氨基甲酸酯类农药及其代谢物残留[J]. 分析实验室, 2019, 38(1): 13-18.
Zhang Y X, Zhang T, Xue X, et al.Simultaneous determination of 17 carbamate pesticides residues in tea by QuEChERS-UPLC-MS/MS[J]. Chinese Journal of Analysis Laboratory, 2019, 38(1): 13-18.
[12] Wang L, Yan T, Zhang K X, et al.A sensitive UPLC-MS/MS method for simultaneous determination of polyphenols and theaflavins in rat plasma: Application to a pharmacokinetic study of Da Hong Pao tea[J]. Biomedical Chromatography, 2019, 33(4): e4470. doi: 10.1002/bmc.4470.
[13] Chen H P, Gao G W, Chai Y F, et al.Multiresidue method for the rapid determination of pesticide residues in tea using ultra performance liquid chromatography orbitrap high resolution mass spectrometry and in-syringe dispersive solid phase extraction[J]. ACS Omega, 2017, 2(9): 5917-5927.
[14] 苏建峰, 钟茂生, 陈晶, 等. 气相色谱-质谱法与气相色谱法测定茶叶及茶叶加工品中295种农药多残留[J]. 分析测试学报, 2015, 34(6): 625-638.
Su J F, Zhong M S, Chen J, et al.Multi-residue determination of 295 pesticides in tea and its products by gas chromatography-mass spectrometry and gas chromatography[J]. Journal of Instrumental Analysis, 2015, 34(6): 625-638.
[15] 陈红平, 刘新, 汪庆华, 等. 气相色谱-质谱法同时测定茶叶中72种农药残留量[J]. 食品科学, 2011, 32(6): 159-164.
Chen H P, Liu X, Wang Q H, et al.Simultaneous determination of 72 pesticide residues in tea by gas chromatography-mass spectrometry[J]. Food Science, 2011, 32(6): 159-164.
[16] 杨尚春, 杨晓云, 宁焕焱, 等. MSPD-GC-μECD快速分析茶叶中己唑醇的残留[J]. 农药, 2010, 49(10): 750-752.
Yang S C, Yang X Y, Ning H Y, et al.Fast analysis of hexaconazole residue in tea by MSPD-GC-μECD[J]. Agrochemicals, 2010, 49(10): 750-752.
[17] 李军明, 钟读波, 王亚琴, 等. 在线凝胶渗透色谱-气相色谱/质谱法检测茶叶中的153种农药残留[J]. 色谱, 2010, 28(9): 840-848.
Li J M, Zhong D B, Wang Y Q, et al.Determination of 153 pesticide residues in tea using on-line gel permeation chromatography-gas chromatography/mass spectrometry[J]. Chinese Journal of Chromatography, 2010, 28(9): 840-848.
[18] 孔维恒, 刘鑫, 云环, 等. 加速溶剂萃取-凝胶渗透色谱-气相色谱质谱测定茶叶中7种农药残留[J]. 分析仪器, 2017, (5): 147-149.
Kong W H, Liu X, Yun H, et al.Determination of seven pesticide residues in tea by GC/MS combined with domestic gel permeation chromatograph cleanup[J]. Analytical Instrumentation, 2017(5): 147-149.
[19] He X, Zhu G, Zheng H, et al.Facile synthesis of polyaniline-coated SiO₂ nanofiber and its application in enrichment of fluoroquinolones from honey samples[J]. Talanta, 2015, 140: 29-35.
[20] Tang S, Lin X H, Li S F Y, et al. In-syringe dispersive solid-phase extraction using dissolvable layered double oxide hollow spheres as sorbent followed by high-performance liquid chromatography for determination of 11 phenols in river water[J]. Journal of Chromatography A, 2014, 1373: 31-39.
[21] Sereshti H, Khodayari F, Nouri N.Integrated in-syringe magnetic sheet solid-phase extraction and dispersive liquid-liquid microextraction for determination of aflatoxins in fresh and moldy breads[J]. Journal of the Science of Food and Agriculture, 2020, 100(3): 1048-1055.
[22] 仲伶俐, 胡莉, 雷绍荣, 等. 超高效液相色谱-串联质谱法测定茶叶中6种农药残留[J]. 食品安全质量检测学报, 2016, 7(5): 2081-2086.
Zhong L L, Hu L, Lei S R, et al.Determination of 6 pesticide residues in tea by ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2016, 7(5): 2081-2086.
[23] 金莉莉, 郝振霞, 高贯威, 等. 超高效液相色谱-静电场轨道阱高分辨质谱法测定茶叶中21种农药残留量[J]. 茶叶科学, 2018, 38(6): 595-605.
Jin L L, Hao Z X, Gao G W, et al.Determination of 21 pesticide residues in tea by ultra performance liquid chromatography orbitrap high resolution mass spectrometry[J]. Journal of Tea Science, 2018, 38(6): 595-605.

Rapid Determination of 24 Pesticide Residues in Tea by in-Syringe Dispersive Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

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