A method for the determination of cyromazine residues in 14 kinds of vegetables including garlic chives by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QQQMS) was established. The samples were extracted with acetonitrile, and then 5 mL supernatant liquid was evaporated with a nitrogen stream and dissolved in 1 mL acetonitrile. The dissolving solution was separated with a hydrophilic chromatography column by isocratic elution using 5 mmol/L ammonium acetate solution containing 0.1% formic acid with acetonitrile as mobile phases. Then, it was detected by electrospray ion source positive ion detection mode and multiple reaction monitoring modes, and quantified by the matrix-matched external standard calibration curves. Cyromazine had a good linear relationship in the concentration range of 0.5-100 μg/L with good correlation coefficients (r>0.99). The average recoveries ranged from 80% to 113% for cyromazine at 3 spiked levels of 2.0, 4.0, and 20.0 μg/kg. The relative standard deviations (RSD, n=3) were in the range of 0.56%-7.21%. The limits of detection were 0.5 μg/kg (S/N=3) and the limits of quantification detection were 2.0 μg/kg(S/N=10).
俞所银
,
闫晴
,
梁佳
. Determination of cyromazine residues in 14 kinds of vegetables by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QQQMS)[J]. Food and Fermentation Industries, 2022
, 48(20)
: 231
-237
.
DOI: 10.13995/j.cnki.11-1802/ts.029826
[1] 黄何何, 吴媛, 徐敦明.液相色谱-串联质谱法测定水果中8种极性农药残留量[J].食品安全质量检测学报, 2018,9(20):5 333-5 339.
HUANG H H, WU Y, XU D M.Determination of 8 kinds of polar pesticides residues in fruits by high performance liquid chromatography-tandem mass spectrometry [J].Journal of Food Safety and Quality, 2018, 9(20):5 333-5 339.
[2] 韩永涛, 张艳峰, 王会利.灭蝇胺在苦瓜上的残留行为及膳食风险评估[J].农药, 2020, 59(6):441-444.
HAN Y T, ZHANG Y F, WANG H L.Residue behavior and dietary risk assessment of cyromazine in bitter gourd [J].Agrochemicals, 2020, 59(6):441-444.
[3] ROOT D S, HONGTRAKUL T, DAUTERMAN W C.Studies on the absorption,residues and metabolism of cyromazine in tomatoes [J].Pesticide Science, 1996,48(1):25-30.
[4] The European agency for the evaluation of medicinal products veterinary medicines and inspections [R].Committee FOR veterinary medicinal Products Cyromazine Summary Report (2), Europ, 2001.
[5] Wikipedia [EB/OL].[2020-04-03].http://en.Wikipedia.org /wiki/Cyanuric acid.
[6] 王京文, 周航, 卜惠斐, 等.灭蝇胺及其代谢物三聚氰胺在大棚黄瓜上的残留降解动态[J].农药, 2011, 50(2):130-132;140.
WANG J W, ZHOU H, BU H F, et al.The degradation dynamics of cyromazine and its metabolite melamine on cucumbers in greenhouse [J].Agrochemicals, 2011, 50(2):130-132;140.
[7] 赵馨. QuEChERS方法在HPLC测定豇豆中灭蝇胺残留量的应用研究[J].福建农业科技,2020(8):7-12.
ZHAO X.Application of the QuEChERS method in the determination of cyromazine residues in cowpeas by HPLC[J].Fujian Agricultural Science and Technology, 2020(8):7-12.
[8] 郝国辉, 颜明, 韩凯, 等.农产品中灭蝇胺检测的基质效应影响分析[J].现代食品, 2021, 27(3):141-144.
HAO G H, YAN M, HAN K, et al.Analysis of the matrix effect on the cyromazine detection in agricultural products[J].Modern Food, 2021, 27(3):141-144.
[9] 张从文, 李红梅.蔬菜中灭蝇胺残留量的液质联用分析方法[J].安徽农学通报, 2018, 24(22):91-95.
ZHANG C W, LI H M.Analysis of cyromazine residues by liquidchromatography-mass spectrometry [J].Anhui Agricultural Science Bulletin, 2018,24(22):91-95.
[10] 田培, 赵慧宇, 刘之炜, 等.杨梅中灭蝇胺及其代谢物检测方法与风险评估[J].浙江农业学报,2021,33(3):534-540.
TIAN P, ZHAO H Y, LIU Z W, et al.Analysis and risk assessment of cyromazine and its metabolites in bayberry [J].Acta Agriculturae Zhejiangensis,2021,33(3):534-540.
[11] 覃国新,劳水兵,李慧玲,等.一步式提取净化/超高效液相色谱-串联质谱法测定水生蔬菜中矮壮素和灭蝇胺[J].食品安全质量检测学报, 2020,11(11):3 619-3 624.
QIN G X, LAO S B, LI H L, et al.Determination of chlormequat and cyromazine residues in aquatic vegetables by ultra performance liquid chromatography-tandem mass spectrometry with extraction and purification on one step[J].Journal of Food Safety and Quality, 2020, 11(11):3 619-3 624.
[12] 谭华东, 赵淑巧, 武春媛.CdSe/CdS量子点荧光探针测定蔬菜中灭蝇胺的残留量[J].分析测试学报, 2019, 38(10):1 207-1 212.
TAN H D, ZHAO S Q, WU C Y.Determination of cyromazine residues in vegetables using a fluorescence probe with CdSe/CdS quantum dots [J].Journal of Instrumental Analysis, 2019, 38(10):1 207-1 212.
[13] 代艳娜, 刘青海, 蒲继锋 , 等.超高效液相色谱-串联质谱法检测芹菜和土壤中灭蝇胺及其代谢物三聚氰胺残留[J].食品安全质量检测学报, 2020, 11(15):5 020-5 026.
DAI Y N, LIU Q H, PU J F, et al.Determination of cyromazine and its metabolite melamine residues in celery and its soil by ultra performance liquid chromatography tandem mass spectrometry[J].Journal of Food Safety and Quality, 2020, 11(15):5 020-5 026.
[14] 徐炜枫. 30 种农产品中灭蝇胺残留检测的基质效应探讨[J].农家致富顾问, 2020(10):238-240.
XU W F.Discussion on the matrix effects of 30 kinds of cyromazine residual detection in agricultural products[J].Farmhouse Get Rich Consultant, 2020(10):238-240.
[15] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 27404—2008实验室质量控制规范 食品理化检测[S]. 北京:中国标准出版社,2008.
The General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China and China National Standardization Management Committee. GB/T 27404—2008 Criterion on quality control of laboratories—Chemical testing of food[S]. Beijing: China Standard Press, 2008.
[16] 杨晋青, 俞所银, 葛宇.QuEChERS-液相色谱-串联质谱法测定南瓜中噻虫胺和氟啶虫胺腈的残留量[J].现代食品科技, 2021, 37(9):319-324.
YANG J Q, YU S Y, GE Y.Determination of clothianidin and sulfoxaflor residues in pumpkin by QuEChERS-liquid chromatography-tandem mass spectrometry[J].Modern Food Science & Technology, 2021, 37(9):319-324.