Determination of 22 Pesticide Residues in Cowpeas and Mangoes by One-step QuEChERS Combined with Ultra Performance Liquid Chromatography-Mass Spectrometry

TONG Kaixuan; XIA Han; LI Jianxun; XIE Yujie; WU Xingqiang; FAN Chunlin; CHEN Hui

doi:10.13386/j.issn1002-0306.2023090002

Volume 45 Issue 17

Aug. 2024

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Science and Technology of Food Industry > 2024 > 45(17): 252-261. > DOI: 10.13386/j.issn1002-0306.2023090002

TONG Kaixuan, XIA Han, LI Jianxun, et al. Determination of 22 Pesticide Residues in Cowpeas and Mangoes by One-step QuEChERS Combined with Ultra Performance Liquid Chromatography-Mass Spectrometry[J]. Science and Technology of Food Industry, 2024, 45(17): 252−261. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023090002.

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Determination of 22 Pesticide Residues in Cowpeas and Mangoes by One-step QuEChERS Combined with Ultra Performance Liquid Chromatography-Mass Spectrometry

1.
Chinese Academy of Inspection and Quarantine, Beijing 100176, China
2.
Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences, Beijing 100193, China

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Received Date: September 04, 2023
Available Online: July 07, 2024

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Abstract

Abstract

A one-step QuEChERS automated detection technology for 22 pesticides in cowpeas and mangoes was established based on ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted by acetonitrile containing 1% acetic acid, added with EN extraction salt (anhydrous Mg₂SO₄, sodium chloride, trisodium citrate dihydrate, disodium hydrogen citrate sesquihydrate) to remove water, and then purified with C₁₈ and graphitized carbon black (GCB). The target analytes were separated by ACQUITY UPLC BEH C₁₈ chromatography column, using 0.01% formic acid aqueous solution (containing 2 mmol/L ammonium formate)-0.01% formic acid methanol as the mobile phase, and determined in multiple reaction monitoring (MRM). The results showed that the 22 pesticides had good linearity in the range of 0.01~25.00 µg/L, with coefficient of determination (R²) higher than 0.994. The limits of detection (LOD, S/N=3) were 0.05~2 µg/kg, and the limits of quantification (LOQ, S/N=10) were 0.1~5 µg/kg. At the spiked levels of 1×LOQ, 2×LOQ, and 10×LOQ, the average recoveries for cowpeas were 70.9%~116.6%, 71.9%~118.3%, and 73.7%~113.7%, respectively, and for mangoes were 70.2%~114.6%, 71.2%~113.7%, and 74.3%~118.5%, respectively. The relative standard deviations for them were all within 20%. The method was successfully applied to the detection of 42 actual samples, and 33 samples detected pesticide residues. This method has high sensitivity and a satisfactory level of automation, effectively reducing human operation steps. It is suitable for the simultaneous detection and accurate quantification of 22 pesticides and their metabolites.
- one-step QuEChERS,
- UPLC-MS/MS,
- pesticide residues,
- cowpea,
- mango

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References

[1]	张群, 段云, 马晨, 等. 豇豆中5种农药及其代谢物残留检测与膳食风险评估[J]. 中国蔬菜,2022(10):86−96. [ZHANG Q, DUAN Y, MA C, et al. Determination of residual quantity from five pesticides and their metabolites in cowpea and dietary risk assessment[J]. China Vegetables,2022(10):86−96.] ZHANG Q, DUAN Y, MA C, et al. Determination of residual quantity from five pesticides and their metabolites in cowpea and dietary risk assessment[J]. China Vegetables, 2022（10）: 86−96.
[2]	马晨, 张群, 刘春华, 等. 海南芒果中农药多残留分析[J]. 农药学学报,2021,23(3):552−560. [MA C, ZHANG Q, LIU C H, et al. Analysis of multiple pesticide residues in mango of Hainan Province[J]. Chinese Journal of Pesticide Science,2021,23(3):552−560.] MA C, ZHANG Q, LIU C H, et al. Analysis of multiple pesticide residues in mango of Hainan Province[J]. Chinese Journal of Pesticide Science, 2021, 23（3）: 552−560.
[3]	YANG B X, MA W, WANG S, et al. Determination of eight neonicotinoid insecticides in Chinese cabbage using a modified QuEChERS method combined with ultra performance liquid chromatography-tandem mass spectrometry[J]. Food Chemistry,2022,387:132935. doi: 10.1016/j.foodchem.2022.132935
[4]	BASS C, DENHOLM I, WILLIAMSON M S, et al. The global status of insect resistance to neonicotinoid insecticides[J]. Pesticide Biochemistry and Physiology,2015,121:78−87. doi: 10.1016/j.pestbp.2015.04.004
[5]	ZHANG Q, XU Y, YING Z, et al. Integrated exposure assessment and potential risks of neonicotinoids in vegetables from three different sources in Zhejiang, China (2018–2020)[J]. Environmental Science and Pollution Research,2023,30(9):22941−22949.
[6]	LI R J, LIU T J, CUI S H, et al. Residue behaviors and dietary risk assessment of dinotefuran and its metabolites in Oryza sativa by a new HPLC-MS/MS method[J]. Food Chemistry,2017,235:188−193. doi: 10.1016/j.foodchem.2017.04.181
[7]	LEE J, KIM J H. Simultaneous analysis of fenthion and its five metabolites in produce using ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Molecules (Basel, Switzerland),2020,25(8):1938. doi: 10.3390/molecules25081938
[8]	PÉREZ-MAYÁN L, RAMIL M, CELA R, et al. Determination of pesticide residues in wine by solid-phase extraction on-line combined with liquid chromatography tandem mass spectrometry[J]. Journal of Food Composition and Analysis,2021,104:104184. doi: 10.1016/j.jfca.2021.104184
[9]	CHEN T, XU H. In vivo investigation of pesticide residues in garlic using solid phase microextraction-gas chromatography-mass spectrometry[J]. Analytica Chimica Acta,2019,1090:72−81. doi: 10.1016/j.aca.2019.09.011
[10]	SAPAHIN H A, MAKAHLEH A, SAAD B. Determination of organophosphorus pesticide residues in vegetables using solid phase micro-extraction coupled with gas chromatography–flame photometric detector[J]. Arabian Journal of Chemistry,2019,12(8):1934−1944. doi: 10.1016/j.arabjc.2014.12.001
[11]	FERNANDES V C, FREITAS M, PACHECO J P G, et al. Magnetic dispersive micro solid-phase extraction and gas chromatography determination of organophosphorus pesticides in strawberries[J]. Journal of Chromatography. A,2018,1566:1−12. doi: 10.1016/j.chroma.2018.06.045
[12]	MOKHTARI S, KHOSROWSHAHI E M, FARAJZADEH M A, et al. Combination of nano-onion-based dispersive solid phase extraction combined with deep eutectic solvent-based dispersive liquid–liquid microextraction for trace analysis of pesticides[J]. Microchemical Journal,2022,183:107983. doi: 10.1016/j.microc.2022.107983
[13]	MIYARDAN F N, AFSHAR MOGADDAM M R, FARAJZADEH M A, et al. Combining modified graphene oxide-based dispersive micro solid phase extraction with dispersive liquid–liquid microextraction in the extraction of some pesticides from zucchini samples[J]. Microchemical Journal,2022,182:107884. doi: 10.1016/j.microc.2022.107884
[14]	张翠芳, 陈兆杰, 宋世明, 等. QuEChERS-超高效液相色谱-串联质谱分析氰霜唑及代谢物CCIM在黄瓜和土壤中的残留[J]. 农药学学报,2018,20(2):204−210. [ZHANG C F, CHEN Z J, SONG S M, et al. Determination of cyazofamid and its metabolite CCIM residue in cucumber and soil with a modified QuEChERS method by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science,2018,20(2):204−210.] ZHANG C F, CHEN Z J, SONG S M, et al. Determination of cyazofamid and its metabolite CCIM residue in cucumber and soil with a modified QuEChERS method by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2018, 20（2）: 204−210.
[15]	朱正伟, 吴婉琴, 朱松松, 等. 高效液相色谱-串联质谱联用技术快速分析水果和蔬菜中毒死蜱及其降解产物[J]. 中国食品卫生杂志,2023,35(1):20−26. [ZHU Z W, WU W Q, ZHU S S, et al. Rapid analysis of chlorpyrifos and its degradation products in fruits and vegetables by HPLC-MS/MS[J]. Chinese Journal of Food Hygiene,2023,35(1):20−26.] ZHU Z W, WU W Q, ZHU S S, et al. Rapid analysis of chlorpyrifos and its degradation products in fruits and vegetables by HPLC-MS/MS[J]. Chinese Journal of Food Hygiene, 2023, 35（1）: 20−26.
[16]	WANG J, HE Z, WANG L, et al. Automatic single-step quick, easy, cheap, effective, rugged and safe sample preparation devices for analysis of pesticide residues in foods[J]. Journal of Chromatography. A,2017,1521:10−18. doi: 10.1016/j.chroma.2017.09.027
[17]	TANKIEWICZ M. Determination of selected priority pesticides in high water fruits and vegetables by modified QuEChERS and GC-ECD with GC-MS/MS confirmation[J]. Molecules (Basel, Switzerland),2019,24(3):417. doi: 10.3390/molecules24030417
[18]	王雅晶, 陈毅, 边姿名, 等. 新型MOFs磁固相萃取-高效液相色谱法测定草莓中2种新烟碱类农药[J]. 中国卫生检验杂志,2023,33(14):1693−1696. [WANG Y J, CHEN Y, BIAN Z M, et al. Determination of two neonicotinoid pesticides in strawberry by novel MOFs magnetic–solid phase extraction–high performance liquid chromatography[J]. Chin J Health Lab Tec,2023,33(14):1693−1696.] WANG Y J, CHEN Y, BIAN Z M, et al. Determination of two neonicotinoid pesticides in strawberry by novel MOFs magnetic–solid phase extraction–high performance liquid chromatography[J]. Chin J Health Lab Tec, 2023, 33（14）: 1693−1696.
[19]	ANĐELKOVIĆ D, BRANKOVIĆ M, KOCIĆ G, et al. Sorbent-excluding sample preparation method for GC-MS pesticide analysis in apple peel[J]. Biomedical Chromatography:BMC,2020,34(1):e4720. doi: 10.1002/bmc.4720
[20]	HARISCHANDRA N R, PALLAVI M S, BHEEMANNA M, et al. Simultaneous determination of 79 pesticides in pigeonpea grains using GC-MS/MS and LC-MS/MS[J]. Food Chemistry,2021,347:128986. doi: 10.1016/j.foodchem.2020.128986
[21]	YANG B, WANG S, MA W, et al. Simultaneous determination of neonicotinoid and carbamate pesticides in freeze-dried cabbage by modified QuEChERS and ultra-performance liquid chromatography-tandem mass spectrometry[J]. Foods (Basel, Switzerland),2023,12(4):699.
[22]	门雪, 吴兴强, 仝凯旋, 等. 改进的QuEChERS法结合液相色谱-高分辨质谱筛查热带水果中33种新烟碱类杀虫剂及杀菌剂[J]. 分析测试学报,2022,41(6):820−826. [MEN X, WU X Q, TONG K X, et al. Screening of 33 neonicotinoid insecticides and fungicides in tropical fruits by liquid chromatography-high resolution mass spectrometry with a modified QuEChERS method[J]. Journal of Instrumental Analysis,2022,41(6):820−826.] MEN X, WU X Q, TONG K X, et al. Screening of 33 neonicotinoid insecticides and fungicides in tropical fruits by liquid chromatography-high resolution mass spectrometry with a modified QuEChERS method[J]. Journal of Instrumental Analysis, 2022, 41（6）: 820−826.
[23]	黄丁宁, 缪丹旎, 赵巧灵, 等. QuEChERS结合超高效液相色谱-串联质谱法同时测定果蔬中12种新烟碱类农药残留[J]. 食品安全质量检测学报,2023,14(9):186−194. [HUANG D N, MIAO D N, ZHAO Q L, et al. Simultaneous determination of 12 kinds of neonicotinoid pesticides in fruits and vegetables by QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety and Quality,2023,14(9):186−194.] HUANG D N, MIAO D N, ZHAO Q L, et al. Simultaneous determination of 12 kinds of neonicotinoid pesticides in fruits and vegetables by QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety and Quality, 2023, 14（9）: 186−194.
[24]	MOL H G J, PLAZA-BOLANOS P, ZOMER P, et al. Toward a generic extraction method for simultaneous determination of pesticides, mycotoxins, plant toxins, and veterinary drugs in feed and food matrixes[J]. Anal Chem,2008,80:9450−9459. doi: 10.1021/ac801557f
[25]	SHU X, CHU N M, ZHANG X M, et al. Rapid analysis of residues of 186 pesticides in Hawk tea using modified QuEChERS coupled with gas chromatography tandem mass spectrometry[J]. Int J Environ Res Pub Health,2022,19(19):12639. doi: 10.3390/ijerph191912639
[26]	LIU T, ZHOU J G, HE L, et al. Determination of polychlorinated biphenyls and organochlorine pesticides in Chinese mitten crabs (Eriocheir sinensis) using modified QuEChERS followed by GC-MS[J]. Anal Method,2020,12(18):2398−2406. doi: 10.1039/D0AY00519C
[27]	LI P P, DUAN Y, GE H L, et al. Multiresidue analysis of 113 pesticides in different maturity levels of mangoes using an optimized QuEChERS method with GC-MS/MS and UHPLC-MS/MS[J]. Food Anal Method,2018,11(10):2742−2757. doi: 10.1007/s12161-018-1263-5
[28]	马智玲, 赵文, 李凌云, 等. 气相色谱-三重四极杆串联质谱法快速测定蔬菜水果中 129 种农药的残留量[J]. 色谱,2013,31(3):228−239. [MA Z L, ZHAO W, LI L Y, et al. Rapid determination of 129 pesticide residues in vegetables and fruits by gas chromatography-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography,2013,31(3):228−239.] doi: 10.3724/SP.J.1123.2012.10029 MA Z L, ZHAO W, LI L Y, et al. Rapid determination of 129 pesticide residues in vegetables and fruits by gas chromatography-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, 2013, 31（3）: 228−239. doi: 10.3724/SP.J.1123.2012.10029
[29]	CHEN D M, YU J, TAO Y F, et al. Qualitative screening of veterinary anti-microbial agents in tissues, milk, and eggs of food-producing animals using liquid chromatography coupled with tandem mass spectrometry[J]. Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences,2016,1017:82−88.
[30]	FERRER C, LOZANO A, ANA A, et al. Overcoming matrix effects using the dilution approach in multiresidue methods for fruits and vegetables[J]. Journal of Chromatography A,2011,1218(42):7634−7639. doi: 10.1016/j.chroma.2011.07.033

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