Determination of Cyhalofop-butyl and Cyhalofop-acid Residues in Cereals and Oilseeds by QuEChERS-UPLC

PENG Hongxia; LIU Ya; YANG Li; LV Xinming; XU Xinzhong; XU Xin; WANG Ke

doi:10.13386/j.issn1002-0306.2021090139

Volume 43 Issue 11

May 2022

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Science and Technology of Food Industry > 2022 > 43(11): 310-317. > DOI: 10.13386/j.issn1002-0306.2021090139

PENG Hongxia, LIU Ya, YANG Li, et al. Determination of Cyhalofop-butyl and Cyhalofop-acid Residues in Cereals and Oilseeds by QuEChERS-UPLC[J]. Science and Technology of Food Industry, 2022, 43(11): 310−317. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021090139.

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Determination of Cyhalofop-butyl and Cyhalofop-acid Residues in Cereals and Oilseeds by QuEChERS-UPLC

1.
College of Food, Shihezi University, Shihezi 832000, China
2.
Technology Center of Alashankou Customs, Alashankou 833418, China
3.
Market Supervision and Administration of Hami City, Hami 839000, China

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Received Date: September 09, 2021
Available Online: April 03, 2022

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Abstract

Objective: The method of QuEChERS-UPLC was established for the simultaneous determination of cyhalofop-butyl and cyhalofop-acid residues in cereals and oilseeds. Methods: The accurately weighed 2.0 g and 5.0 g sample was extracted with 0.1% formic acid water-acetonitrile (1:1, V/V) as extractant, and then purified with dispersive solid phase extraction adsorbents, such as N-propyl ethylenediamine (PSA), C₁₈, sodium chloride, anhydrous magnesium sulfate, etc. After the purified solution was filtered through a 0.22 μm filter membrane, it was eluted with 0.1% phosphoric acid aqueous solution-methanol-acetonitrile as the mobile phase for gradient elution, separated by ACQUITY UPLC BEH C₁₈ (50 mm × 2.1 mm, 1.7 μm) chromatographic column, analyzed and detected by UPLC, and quantified by external standard method. Results: In the range of 0.002~5 μg/mL, the mass concentration of cyhalofop-butyl and cyhalofop-acid showed a good linear relationship with the peak area, and the limits of quantification in grains and oilseeds were 0.01 mg/kg and 0.02 mg/kg, respectively. The recoveries of cyhalofop-butyl and cyhalofop-acid in cereals were 89.23%~101.12% and 87.98%~100.02%. Those in oilseeds were 85.12%~92.34% and 82.63%~89.55% respectively. The relative standard deviation was 1.1%~3.3%. Conclusion: The method used in this experiment has a simple pretreatment process, accurate and efficient detection process, and its sensitivity and accuracy meet the requirements of pesticide residue detection. It is suitable for the detection of cyhalofop-butyl and cyhalofop-acid residues in grains and oilseeds.
- cyhalofop-butyl,
- cyhalofop-acid,
- UPLC,
- QuEChERS,
- pesticide residue

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[1]	闫潇敏, 宁斌科, 王列平. 新型选择性除草剂-氰氟草酯的开发与使用[J]. 世界农药,2007(2):43−45. [YAN X M, NING B K, W L P. New selective herbicide-development and application of cyhalofop-butyl[J]. World Pesticide,2007(2):43−45. doi: 10.3969/j.issn.1009-6485.2007.02.011
[2]	黄晓华, 肖鸣, 郑爱妹. 氰氟草酯及其同系衍生物的分离与测定[J]. 农药科学与管理,2016,37(10):44−48. [HUANG X H, XIAO M, ZHENG A M. Separation and determination of cyhalofop-butyl and its homologous derivatives[J]. Pesticide Science and Management,2016,37(10):44−48. doi: 10.3969/j.issn.1002-5480.2016.10.012
[3]	PINNA M V, BRASCHI I, BLASIOLI S, et al. Hydrolysis and adsorption of cyhalofop-butyl and cyhalofop-acid on soil coll-oids[J]. Journal of Agricultural and Food Chemistry,2008,56(13):5273−5277. doi: 10.1021/jf800542b
[4]	魏凤, 杨仁斌, 蒋波, 等. 高效液相色谱法测定稻田中氰氟草酯[J]. 环境监测管理与技术,2015,27(5):45−48. [WEI F, YANG R B, JIANG B, et al. Determination of cyhalofop-butyl in paddy fields by HPLC[J]. Environmental Monitoring Management and Technology,2015,27(5):45−48. doi: 10.3969/j.issn.1006-2009.2015.05.012
[5]	WANG L C, HSI H C, CHANG J E, et al. Influence of start-up on PCDD/F emission of incinerators[J]. Chemosphere,2007,67(7):1346−1353. doi: 10.1016/j.chemosphere.2006.10.081
[6]	JÜRGEN R, ROLAND W, ROLAND H. Long-term monitoring of PCDD/PCDF and other unintentionally produced POPs-Concepts and case studies from Europe[J]. Science China (Chemistry),2010,53(5):1017−1024.
[7]	KUMAR B, SHARMA R, SINGH S B. Evaluation of harvest residues of cyhalofop-butyl in paddy soil[J]. Bulletin of Environmental Contamination and Toxicology,2012,89(2):344−347. doi: 10.1007/s00128-012-0701-0
[8]	WU N, ZHAO L X, JIANG C Y, et al. A naked-eye visible colorimetric and fluorescent chemosensor for rapid detection of fluoride anions: Implication for toxic fluorine-containing pesticides detection[J]. Journal of Molecular Liquids,2020,302:112549. doi: 10.1016/j.molliq.2020.112549
[9]	赵莉, 朱国念, 姜忠涛. 氰氟草酯及其代谢物在稻田水、土壤和稻株中的残留分析方法[J]. 分析化学,2003(2):163−166. [ZHAO L, ZHU G N, JIANG Z T. Residue analysis method of cyhalofop-butyl and its metabolites in paddy water, soil and rice plants[J]. Analytical Chemistry,2003(2):163−166. doi: 10.3321/j.issn:0253-3820.2003.02.008
[10]	李向阳, 倪立霞, 姜士聚, 等. 9%嘧肟·氰氟草乳油高效液相色谱分析[J]. 农药,2019,58(11):816−818,823. [LI X Y, NI L X, JIANG S J, et al. Analysis of 9% azoxime·cyhalothrin EC by HPLC[J]. Pesticide,2019,58(11):816−818,823.
[11]	SOLIMAN M, KHORSHID M A, EL-MARSAFY A M, et al. Determination of 10 pesticides, newly registered in Egypt, using modified QuEChERS method in combination with gas and liquid chromatography coupled with tandem mass spectrometric detec-tion[J]. International Journal of Environmental Analytical Chemistry,2019,99(3):224−242. doi: 10.1080/03067319.2019.1588263
[12]	WANG J D, BAO H J, SHI H Y, et al. Development of an enzyme-linked immunosorbent assay for quantitative determination of cyhalofop-butyl[J]. Pesticide Biochemistry and Physiology,2010,98(1):68−72. doi: 10.1016/j.pestbp.2010.05.001
[13]	张乐, 赵文文, 郭静远, 等. 水稻中除草剂氯氟吡氧乙酸异辛酯和氰氟草酯的检测方法及其储藏稳定性研究[J]. 食品安全质量检测学报,2021,12(15):5923−5930. [ZHANG L, ZHAO W W, GUO J Y, et al. Study on the determination method and storage stability of herbicides isooctyl chlorofluoropyroxyacetate and cyhalofop-butyl in rice[J]. Journal of Food Safety and Quality Testing,2021,12(15):5923−5930.
[14]	徐永丙, 滕菲菲, 李婷婷, 等. 20%五氟·唑·氰氟可分散油悬浮剂及其代谢物在稻田中的残留与消解[J]. 农药,2020,59(9):670−675. [XU Y B, TENG F F, LI T T, et al. Residue and digestion of 20% pentafluoro·oxazole·cyanofluoride dispersible oil suspension and its metabolites in paddy field[J]. Pesticide,2020,59(9):670−675.
[15]	贾小晴. 植物源性食品中氟啶胺检测方法的研究[D]. 长春: 吉林大学, 2017 JIA X Q. Study on the detection method of fluazinam in plant derived foods[D]. Changchun: Jilin University, 2017.
[16]	董婷, 罗泽江. 超高效液相色谱法测定稻田水和土壤中氰氟草酯及其代谢产物[J]. 广州化工,2017,45(20):100−102. [DONG T, LUO Z J. Determination of cyhalofop-butyl and its metabolites in paddy water and soil by UPLC[J]. Guangzhou Chemical Industry,2017,45(20):100−102. doi: 10.3969/j.issn.1001-9677.2017.20.035
[17]	孙明娜, 王梅, 余璐, 等. 基质分散固相-液质联用法检测稻田水和土壤中氰氟草酯和双草醚残留[J]. 环境化学,2017,36(3):691−694. [SUN M N, WANG M, YU L, et al. Determination of cyhalofop-butyl and bisoxyfen residues in paddy water and soil by matrix dispersion solid phase liquid mass spectrometry[J]. Environmental Chemistry,2017,36(3):691−694. doi: 10.1002/etc.3570
[18]	ANASTASSIADES M, LEHOTAY S J, ŠTAJNBAHER D, et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce[J]. Journal of AOAC International,2019,86(2):412−431.
[19]	孟志娟, 黄云霞, 赵丽敏, 等. 气相色谱-串联质谱法测定水果中50种农药残留[J]. 色谱,2018,36(9):917−924. [MENG Z J, HUANG Y X, ZHAO L M, et al. Determination of 50 pesticide residues in fruits by gas chromatography-tandem mass spectrometry[J]. Chromatography,2018,36(9):917−924.
[20]	李晔, 赵丹莹, 郭爱华, 等. 分散固相萃取-气相色谱-三重四级杆串联质谱法测定代用茶中14种农药残留[J]. 卫生研究,2018,47(4):621−627. [LI Y, ZHAO D Y, GUO A H, et al. Determination of 14 pesticide residues in substitute tea by dispersive solid phase extraction-gas chromatography-triple quadrupole tandem mass spectrometry[J]. Health Research,2018,47(4):621−627.
[21]	蓝梦哲, 林绪, 刘雅琼, 等. 液相色谱-串联质谱法同时测定8种花草茶中77种农药残留[J]. 色谱,2018,36(9):938−945. [LAN M Z, LIN X, LIU Y Q, et al. Simultaneous determination of 77 pesticide residues in 8 kinds of herbal teas by liquid chromatography tandem mass spectrometry[J]. Chromatography,2018,36(9):938−945.
[22]	HOU X, LEI S, QIU S, et al. A multi-residue method for the determination of pesticides in tea using multi-walled carbon nanotubes as a dispersive solid phase extraction absorbent[J]. Food Chemistry,2014,153:121−129. doi: 10.1016/j.foodchem.2013.12.031
[23]	WILKOWSKA A, BIZIUK M. Determination of pesticide residues in food matrices using the QuEChERS methodology[J]. Food Chemistry,2011,125(3):803−812. doi: 10.1016/j.foodchem.2010.09.094
[24]	李菊颖, 何健, 豆叶枝, 等. 分散固相萃取-液相色谱质谱法测定多种基质中的氰氟草酯和氰氟草酸[J]. 化学研究与应用,2019,31(1):160−165. [LI J Y, HE JIAN, DOU Y Z, et al. Determination of cyhalofop-butyl and cyhalofop-acid in various substrates by dispersive solid phase extraction-liquid chromatography mass spectrometry[J]. Chemical Research and Application,2019,31(1):160−165. doi: 10.3969/j.issn.1004-1656.2019.01.026
[25]	王晓玉, 戈大庆, 潘金菊, 等. 噁唑酰草胺和氰氟草酯在水稻中的残留及膳食风险评估[J]. 农药科学与管理,2021,42(1):39−44, 49. [WANG X Y, GE D Q, PAN J J, et al. Residue and dietary risk assessment of oxazolyl oxalamide and cyhalofop-butyl in rice[J]. Pesticide Science and Management,2021,42(1):39−44, 49. doi: 10.3969/j.issn.1002-5480.2021.01.009
[26]	WU J, WANG K, ZHANG Y, et al. Determination and study on dissipation and residue determination of cyhalofop-butyl and its metabolite using HPLC-MS/MS in a rice ecosystem[J]. Environmental Monitoring and Assessment,2014,186(10):6959−6967. doi: 10.1007/s10661-014-3902-7
[27]	郝经文, 徐文冬, 石敏珠, 等. GC-MS同时测定霍山石斛及霍山产铁皮石斛中拟除虫菊酯和氨基甲酸酯类16种农药残留的检测方法[J]. 食品工业科技,2019,40(9):230−234. [HAO J W, XU W D, SHI M Z, et al. Simultaneous determination of 16 pyrethroid and carbamate pesticide residues in Dendrobium huoshanense and Dendrobium candidum from Huoshan by GC-MS[J]. Food Industry Science and Technology,2019,40(9):230−234.
[28]	周霞, 陈万勤, 陈晶燕, 等. QuEChERS-高效液相色谱-串联质谱法测定春笋中4种农药残留[J]. 中国食品卫生杂志,2018,30(5):486−490. [ZHOU X, CHEN W Q, CHEN J Y, et al. Determination of four pesticide residues in spring bamboo shoots by QuEChERS-HPLC-MS/MS[J]. Chinese Journal of Food Hygiene,2018,30(5):486−490.
[29]	孟繁磊, 宋志峰, 张振都, 等. 超高液相色谱法测定黄瓜中的4种苯并咪唑类农药残留量[J]. 吉林农业,2017(22):62,72. [MENG F L, SONG Z F, ZHANG Z D, et al. Determination of four benzimidazole pesticide residues in cucumber by UPLC[J]. Jilin Agriculture,2017(22):62,72.
[30]	杨路平, 邵立君, 王国玲, 等. QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留[J]. 食品工业科技,2019,40(14):247−253. [YANG L P, SHAO L J, WANG G L, et al. Determination of 13 pesticide residues in edible fungi by QuEChERS combined with liquid chromatography tandem mass spectrometry[J]. Food Industry Science and Technology,2019,40(14):247−253.
[31]	LEHOTAY S J, MASTOVSKA K, LIGHTFIELD A R, et al. Multi-analyst, multi-matrix performance of the QuEChERS approach for pesticide residues in foods and feeds using HPLC/MS/MS analysis with different calibration techniques[J]. Journal of AOAC International,2010,93(2):355−367. doi: 10.1093/jaoac/93.2.355
[32]	GARRIDO FRENICH A, GONZÁLEZ-RODRÍGUEZ M J, ARREBOLA F J, et al. Potentiality of gas chromatography-triple quadrupole mass spectrometry in vanguard and rearguard methods of pesticide residues in vegetables[J]. Analytical Chemistry,2005,77(14):4640−4648. doi: 10.1021/ac050252o
[33]	DA COSTA MORAIS E H, COLLINS C H, JARDIM I C S F. Pesticide determination in sweet peppers using QuEChERS and LC-MS/MS[J]. Food Chemistry,2018,249:77−83. doi: 10.1016/j.foodchem.2017.12.092
[34]	赵莉, 樊晓青, 朱国念. 氰氟草酯水解动力学研究[J]. 农药学学报,2009,11(2):274−278. [ZHAO L, FAN X Q, ZHU G N. Study on hydrolysis kinetics of cyhalothrin[J]. Journal of Pesticide Science,2009,11(2):274−278. doi: 10.3969/j.issn.1008-7303.2009.02.022
[35]	秦姗姗. 农产品中农药残留分析方法研究及基质效应探讨[D]. 郑州: 郑州大学, 2015 QIN S S. Study on analytical methods of pesticide residues in agricultural products and discussion on matrix effects[D]. Zhengzhou: Zhengzhou University, 2015.
[36]	陈国峰, 尤红梅, 滕瑶, 等. UPLC-MS/MS法测定水稻中噁唑酰草胺和氰氟草酯及其代谢物的残留及膳食风险评估[J]. 中国稻米,2021,27(2):57−62. [CHEN G F, YOU H M, TENG Y, et al. Determination of oxazolyl oxalamide, cyhalofop-butyl and their metabolites in rice by UPLC-MS/MS and dietary risk assessment[J]. China Rice,2021,27(2):57−62. doi: 10.3969/j.issn.1006-8082.2021.02.012
[37]	HUANG Y, SHI T, LUO X, et al. Determination of multi-pesticide residues in green tea with a modified QuEChERS protocol coupled to HPLC-MS/MS[J]. Food Chemistry,2019,275:255−264. doi: 10.1016/j.foodchem.2018.09.094
[38]	赵志高, 付延伟, 秦家安, 等. Qu EchERS前处理法联合气相色谱串联质谱检测法快速定量分析甘草中34种农药残留[J]. 中国中药杂志,2019,44(23):5094−5101. [ZHAO Z G, FU Y W, QIN J A, et al. Rapid quantitative analysis of 34 pesticide residues in licorice by QuEchERS pretreatment combined with gas chromatography tandem mass spectrometry[J]. Chinese Journal of Traditional Chinese Medicine,2019,44(23):5094−5101.
[39]	叶学敏. 新型QuEChERS方法在果蔬农残分析中的应用研究[D]. 杭州: 浙江工业大学, 2020 YE X M. Application of the new QuEChERS method in the analysis of agricultural residues in fruits and vegetables[D]. Hangzhou: Zhejiang University of Technology, 2020.
[40]	甘静妮, 程雪梅, 莫晓君, 等. 分散固相萃取/气相色谱-三重四极杆串联质谱测定蔬菜和水果中67种农药残留[J]. 分析测试学报,2016,35(12):1528−1534. [GAN J N, CHENG X M, MO X J, et al. Determination of 67 pesticide residues in vegetables and fruits by dispersive solid phase extraction/gas chromatography-triple quadrupole tandem mass spectrometry[J]. Journal of Analysis and Testing,2016,35(12):1528−1534. doi: 10.3969/j.issn.1004-4957.2016.12.003

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Science and Technology of Food Industry

Determination of Cyhalofop-butyl and Cyhalofop-acid Residues in Cereals and Oilseeds by QuEChERS-UPLC

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