SHAO Ying, ZHANG Hongwei, GAO Ruigang, et al. Simultaneous Screening of 90 Pesticides in Blueberry by Ultra-high Pressure Liquid Chromatography Coupled to High Resolution Mass Spectrometry[J]. Science and Technology of Food Industry, 2023, 44(5): 230−240. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022040026.
Citation: SHAO Ying, ZHANG Hongwei, GAO Ruigang, et al. Simultaneous Screening of 90 Pesticides in Blueberry by Ultra-high Pressure Liquid Chromatography Coupled to High Resolution Mass Spectrometry[J]. Science and Technology of Food Industry, 2023, 44(5): 230−240. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022040026.

Simultaneous Screening of 90 Pesticides in Blueberry by Ultra-high Pressure Liquid Chromatography Coupled to High Resolution Mass Spectrometry

More Information
  • Received Date: April 05, 2022
  • Available Online: January 02, 2023
  • A method for simultaneous screening of 90 pesticide residues in blueberries by ultra-high pressure liquid chromatography high resolution mass spectrometry was developed. Target residues in blueberries were extracted by an improved QuEChERS protocol. Ultra-high pressure liquid chromatography coupled to quadrupole/orbitrap high-resolution mass spectrometry was employed for screening analysis with full mass scanning trigged data dependent fragment ion acquisition in positive and negative mode. The analytes were quantified by representative matrix-matched standard curve. The results showed that the optimized ratio of PSA vs C18 was 1:1 with amount of 150 mg respectively in the improved QuEChERS protocol. The limits of detection and limits of quantitation of the method were 0.1~18.7 μg/kg and 0.2~20.2 μg/kg as well. The linearities for 90 pesticides were fitted by regression calculation at the range of 0.005~0.1 mg/kg with determination coefficient R2≥0.992. With calibration of the representative matrix-matched standard curve, recoveries were calculated ranging from 50.1% to 130.9% and relative standard deviations were varied in the scope of 1.0%~14.9% at the three spiking levels of 0.01, 0.05 and 0.1 mg/kg. Five pesticides were detected in the real-life blueberry samples purchased in the market, evidencing the applicability of the developed method. The proposed approach is applicable for routine pesticide monitoring in blueberries with simple sample preparation, broad analyte coverage and powerful capability of quantification and qualification.
  • [1]
    唐颖. 高铵胁迫对土壤性质、蓝莓苗生长及生理的影响[D]. 大连: 大连理工大学, 2018

    TANG Ying. Effects of high ammonium stress on soil properties, growth and physiology of blueberry seedlings[D]. Dalian: Dalian University of Technology, 2018.
    [2]
    张佳. 北高丛蓝莓内在品质评价研究[D]. 北京: 中国农业科学院, 2020

    ZHANG Jia. Research on inner quality evaluation of Northern highbush blueberry[D]. Beijing: Chinese Academy of Agricultural Sciences Thesis, 2020.
    [3]
    中华人民共和国国家卫生健康委员会, 中华人民共和国农业农村部, 国家市场监督管理总局. GB 2763-2019食品安全国家标准 食品中农药最大残留限量[S]. 北京: 中国农业出版社, 2019.

    The State Health Commission of the People's Republic of China, The Ministry of Agriculture and Rural Areas of the People's Republic of China, The State Market Supervision and Administration. GB 2763-2019 National Food Safety Standard-Maximum residue limits of pesticides in food[S]. Beijing: China Agriculture Press, 2019.
    [4]
    中华人民共和国国家卫生健康委员会, 中华人民共和国农业农村部, 国家市场监督管理总局. GB 2763-2019食品安全国家标准 食品中农药最大残留限量[S]. 北京: 中国农业出版社, 2021

    The State Health Commission of the People's Republic of China, The Ministry of Agriculture and Rural Areas of the People's Republic of China, The State Market Supervision and Administration. GB 2763-2021 National Food Safety Standard-Maximum residue limits of pesticides in food[S]. Beijing: China Agriculture Press, 2021.
    [5]
    嬴金鹏, 王绪凤. 快速检测农残方法的研究[J]. 食品安全导刊,2021,9(84):153−154. [YING Jinpeng, WANG Xufeng. Study on rapid detection of pesticide residues[J]. China Food Safety Magazine,2021,9(84):153−154.
    [6]
    李婷婷, 朱璐, 李玲. 果蔬中农药残留检测方法浅析[J]. 食品安全导刊,2021,18(59):102−103. [LI Tingting, ZHU Lu, LI Ling. Analysis on detection methods of pesticide residues in fruits and vegetables[J]. China Food Safety Magazine,2021,18(59):102−103.
    [7]
    刘渊, 朱虎, 高迎利. 食品中快速检测农药残留技术探究[J]. 食品安全导刊,2021,15(89):158−160. [LIU Yuan, ZHU Hu, GAO Yingli. Research on rapid detection of pesticide residues in food[J]. China Food Safety Magazine,2021,15(89):158−160.
    [8]
    朱仁萍. 果蔬中农药多组分残留的检测方法研究[J]. 食品安全导刊,2020,36(104):167−168. [ZHU Renping. Study on detection method of pesticide multicomponent residues in fruits and vegetables[J]. China Food Safety Magazine,2020,36(104):167−168.
    [9]
    HELEN S, KITTLAUS S, KEMPE G, et al. Reduction of matrix effects in liquid chromatography−electrospray ionization−mass spectrometry by dilution of the sample extracts: How much dilution is needed?[J]. Analytical Chemistry,2012,84(3):1474−1482. doi: 10.1021/ac202661j
    [10]
    SAVINII S, BANDINI M, SANNINO A. An improved, rapid, and sensitive ultra-high-performance liquid chromatography-high-resolution Orbitrap mass spectrometry analysis for the determination of highly polar pesticides and contaminants in processed fruits and vegetables[J]. Journal of Agricultural and Food Chemistry,2019,67(9):2716−2722. doi: 10.1021/acs.jafc.8b06483
    [11]
    吴建霞, 梁小刚, 王垄, 等. QuEChERS-三重四极杆气质联用法测定蓝莓中192种农药残留[J]. 酿酒科技,2021,8(326):118−125. [WU Jianxia, LIANG Xiaogang, WANG Long, et al. Determination of 192 pesticide residues in blueberry by QuEChERS-GS-MS/MS[J]. Liquor-making Science & Technology,2021,8(326):118−125.
    [12]
    李长滨, 杨盛茄, 杨谨旭, 等. QuEChERS-LC-MS/MS联用技术对浆果中多种农药残留的测定[J]. 中国酿造,2019,38(7):174−177. [LI Changbin, YANG Shengru, YANG Jinxu, et al. Determination of multiple pesticide residues in berries by QuEChERS combined with LC-MS/MS[J]. China Brewing,2019,38(7):174−177.
    [13]
    NATALIA B, CESIO V, HEINZEN H, et al. Matrix effects and interferences of different citrus fruit coextractives in pesticide residue analysis using ultrahigh-performance liquid chromatography-high resolution mass spectrometry[J]. Journal of Agricultural and Food Chemistry,2017,65(23):4819−4829. doi: 10.1021/acs.jafc.7b00243
    [14]
    吴学进, 刘春华, 罗金辉, 等. QuEChERS净化—超高效液相色谱—串联质谱法同步测定荔枝中10种植物生长调节剂残留[J]. 南方农业学报,2020,51(10):2532−2539. [WU Xuejin, LIU Chunhua, LUO Jinhui, et al. Simultaneous determination of ten plant growth regulators residues in litchi by QuEChERS clean up-ultra high performance liquid chromatography-tandem mass spectrometr[J]. Journal of Southern Agriculture,2020,51(10):2532−2539.
    [15]
    LUPO S A, ROMESBERG R L, LU X. Automated inline pigment removal for the analysis of pesticide residues in spinach by liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography A,2020,1629:461−477.
    [16]
    NATALIA M, LUANA F, MAIARA S, et al. Determination of pesticide residues in golden berry (Physalis peruviana L.) by modified QuEChERS method and ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry[J]. Food Analytical Methods,2017,10(2):320−329. doi: 10.1007/s12161-016-0582-7
    [17]
    平新亮, 林媚, 姚周麟, 等. 杨梅中36种农药残留快速检测技术研究[J]. 食品科技,2020,45(5):328−333. [PING Xinliang, LIN Mei, YAO Zhoulin, et al. Study on rapid detection of 36 pesticide residues in Myrica rubra[J]. Food Science and Technology,2020,45(5):328−333.
    [18]
    刘华文, 苏海雁, 陆小康, 等. QuEChERS/超高效液相色谱-串联质谱法测定茶叶中28种农药残留[J]. 食品工业科技,2021,42(2):223−229. [LIU Huawen, SU Haiyan, LU Xiaokang, et al. Determination of 28 kinds of pesticide residues in tea by QuEChERS/ultra performance liquid chromatography-tandem mass spectrometry[J]. Science and Technology of Food Industry,2021,42(2):223−229.
    [19]
    PUGAJEVA I, IKKERE L E, JUDJALLO E, et al. Determination of residues and metabolites of more than 140 pharmacologically active substances in meat by liquid chromatography coupled to high resolution Orbitrap mass spectrometry[J]. Journal of Pharmaceutical and Biomedical Analysis,2019,166:252−263. doi: 10.1016/j.jpba.2019.01.024
    [20]
    VALERA-TARIFA N M, SANTIAGO-VALVERDE R, HERNÁNDEZ-TORRES E, et al. Development and full validation of a multiresidue method for the analysis of a wide range of pesticides in processed fruit by UHPLC-MS/MS[J]. Food Chemistry,2020,315:226−304.
    [21]
    司露露, 梁杨琳, 吕春秋, 等. QuEChERS-气相色谱-串联质谱法和高效液相色谱-串联质谱法快速检测蔬菜中267种香港规例中的农药残留量[J]. 食品安全质量检测学报,2021,12(1):122−136. [SI Lulu, LIANG Yanglin, LYU Chunqiu, et al. Rapid determination of 267 kinds of Hong Kong regulatory pesticide residues in vegetables by QuEChERS combined with gas chromatography-tandem mass spectrometry and high performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety and Quality,2021,12(1):122−136.
    [22]
    SUN R, YANG W, LI Y, et al. Multi-residue analytical methods for pesticides in teas: A review[J]. European Food Research and Technology,2021,247(8):1839−1858. doi: 10.1007/s00217-021-03765-3
    [23]
    KWON H, LEHOTAY S J, L GEIS-ASTEGGIANTE. Variability of matrix effects in liquid and gas chromatography-mass spectrometry analysis of pesticide residues after QuEChERS sample preparation of different food crops[J]. Journal of Chromatography A,2012,12(7):235−245.
    [24]
    GUO Z, ZHU Z, HUANG S, et al. Non-targeted screening of pesticides for food analysis using liquid chromatography high-resolution mass spectrometry-A review[J]. Food Additives & Contaminants,2020,37(7):1180−1201.
    [25]
    梁秀美, 张维一, 张微, 等. QuEChERS-HPLC-MS/MS法同时测定水果中38种农药的残留量[J]. 食品科学,2021,41(8):288−296. [LIANG Xiumei, ZHANG Weiyi, ZHANG Wei, et al. Simultaneous determination of residues of 38 pesticides in fruits by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry[J]. Food Science,2021,41(8):288−296.
    [26]
    SONG N, MIYOUNG Y, TAE G N. Multi-residue analysis of 203 pesticides in strawberries by liquid chromatography tandem mass spectrometry in combination with the QuEChERS method[J]. CYTA: Journal of Food,2019,17(1):976−987. doi: 10.1080/19476337.2019.1680579
    [27]
    袁瑷金, 崔凌峰. QuEChERS前处理方法在食品检测中的应用[J]. 分析检测,2020(12):173−175. [YUAN Aijin, CUI Lingfeng. Application of QuEChERS pretreatment method in food testing[J]. Analysis and Testing,2020(12):173−175.
    [28]
    CHAMKASEM N. Rapid determination of polar pesticides and plant growth regulators in fruits and vegetables by liquid chromatography-tandem mass spectrometry[J]. J Environ Sci Health B,2018,53(9):622−631. doi: 10.1080/03601234.2018.1473977
    [29]
    WANG Z, CHANG Q, KANG J, et al. Screening and identification strategy for 317 pesticides in fruits and vegetables by liquid chromatography-quadrupole time-of-flight high resolution mass spectrometry[J]. Analytical Methods,2015,7(15):6385−6402. doi: 10.1039/C5AY01478F
    [30]
    CASADO J, BRIGDEN K, SANTILLO D, et al. Screening of pesticides and veterinary drugs in small streams in the European Union by liquid chromatography high resolution mass spectrometry[J]. Science of the Total Environment,2019,6(7):1204−1225.
  • Related Articles

    [1]MENG Hu, LI Yuanjin, ZHAO Danni, ZHANG Yating, ZHANG Dan, YANG Qi, FENG Xinyi. Determination of 21 Triazole Fungicides in Fruits and Vegetables by Lipophilicity-matched Chromatographic Separation-Ultra Performance Liquid Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2024, 45(3): 293-301. DOI: 10.13386/j.issn1002-0306.2023040271
    [2]LI Tingting, WANG Rong, REN Xingquan, LIU Pan, CHEN Kun, HUO Wenqing, ZENG Wenjin. Determination of 26 Kinds of Organophosphorus Pesticide Residues in Wheat Germ by Gas Chromatography Method Simultaneously[J]. Science and Technology of Food Industry, 2023, 44(1): 307-315. DOI: 10.13386/j.issn1002-0306.2022030290
    [3]ZHANG Jin-jun, XIA Hui-li, GAO Hai-bo. Determination of 6 Kinds of Fluoroquinolones in Bean Sprouts Based on Dispersed Solid Phase Extraction UPLC-MS/MS Method[J]. Science and Technology of Food Industry, 2020, 41(23): 260-265,271. DOI: 10.13386/j.issn1002-0306.2020020288
    [4]ZHANG Hong-yan, QIU Guo-yu, WU Fu-xiang, XU Xiao-hui, LI Chen-xi, PAN Xiu-li, WANG Xiao-qiao. Determination of Sulfonamides in Animal-originated Foods by Grinder-QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry and Research on Matrix Effects[J]. Science and Technology of Food Industry, 2020, 41(10): 259-264,270. DOI: 10.13386/j.issn1002-0306.2020.10.043
    [5]ZHOU Ting-ting, CHEN Lu-tao, ZHOU Min, YU Lu-ping, LIU Xiao-yu, LI Bin, HU Jin-feng, ZHU Meng-meng. Determination of Ethephon Residues in Fruits and Vegetables by Gas Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2019, 40(15): 201-206,214. DOI: 10.13386/j.issn1002-0306.2019.15.033
    [6]ZHOU Chun-jie, HOU Mei-ling, HE Chun-lan, LIU Huan, YANG Xiao-shan. Progress on Application of LC-MS/MS Technology in Pesticide Multiresidue Analysis for Food[J]. Science and Technology of Food Industry, 2019, 40(13): 283-286,298. DOI: 10.13386/j.issn1002-0306.2019.13.047
    [7]JIA Qing-hua, HAN Ai-zhi, XI Qian, WANG Zi-kun, LI Ya-wen. Matrix effects of 9 industrial dyes in foods by high performance liquid chromatography with gelpermeation chromatography purification[J]. Science and Technology of Food Industry, 2018, 39(5): 268-271,279.
    [9]ZHAO Guo-zhong, WANG Meng-ying, YAO Yun-ping, HAN Jun-yan, CHEN Wei. Screening of salt tolerant lactic acid bacteria in soy sauce fermentation and its effect on the quality of soy sauce[J]. Science and Technology of Food Industry, 2015, (13): 184-188. DOI: 10.13386/j.issn1002-0306.2015.13.030
    [10]NIE Xi-du, FU Liang. Determination of heavy metal elements in food antcaking agent sodium aluminosilicate by inductively coupled plasma mass spectrometry[J]. Science and Technology of Food Industry, 2015, (12): 57-60. DOI: 10.13386/j.issn1002-0306.2015.12.003
  • Cited by

    Periodical cited type(0)

    Other cited types(3)

Catalog

    Article Metrics

    Article views (229) PDF downloads (28) Cited by(3)

    /

    DownLoad:  Full-Size Img  PowerPoint
    Return
    Return