A method was developed for the determination of amitraz (AMZ), chlordimeform, and their metabolites residues in honey by dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem.2 g honey sample was fully infiltrated with 10 mL aqueous solution and ultrasonic-assisted extraction with 1% ammonium hydroxide-acetonitrile followed by centrifugation, and then cleaned-up by PSA, C18, and NH2, the target compounds were analyzed by ACQUITY UPLC BEH C18 (2.1 mm×50 mm, 1.7 μm) column using a mixture of methanol and 0.1% formic acid aqueous solution as mobile phases with gradient elution, the mass spectrometer was operated under MRM mode in positive mode.The average recoveries of 6 pesticides and metabolites were in the range of 84.1%-113.8%, and the relative standard deviation (RSD) was in the range of 0.9%-6.0%, the limit of detection was between 0.2 μg/kg and 0.8 μg/kg and the limit of quantification was between 0.7 μg/kg and 2.5 μg/kg for target pesticides, respectively.This method was simple, quick, high sensitivity, and could be used for the routine analysis of amitraz, chlordimeform, and their metabolites residues in honey.
WANG Li
,
WEI Maoqiong
,
KANG Hongyu
,
CHEN Xinglian
,
LAN Shanshan
,
ZHANG Xueyan
,
LIU Hongcheng
. Determination of amitraz, chlordimeform, and their metabolites in honey by dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Food and Fermentation Industries, 2024
, 50(8)
: 284
-289
.
DOI: 10.13995/j.cnki.11-1802/ts.036706
[1] TERZO S, MULÈ F, AMATO A. Honey and obesity-related dysfunctions: A summary on health benefits[J]. The Journal of Nutritional Biochemistry, 2020, 82:108401.
[2] SOARES S, AMARAL J S, OLIVEIRA M B P P, et al. A comprehensive review on the main honey authentication issues: Production and origin[J]. Comprehensive Reviews in Food Science and Food Safety, 2017, 16(5):1072-1100.
[3] UGUSMAN A, SHAHRIN S A S, AZIZAN N H, et al. Role of honey in obesity management: A systematic review[J]. Frontiers in Nutrition, 2022, 9:924097.
[4] 谭璟慧, 谢宏斌, 李贵荣, 等. 超高效液相色谱法同时测定蜂蜜中双甲脒及其代谢物残留量[J]. 食品安全质量检测学报, 2020, 11(12):4091-4096.
TAN J H, XIE H B, LI G R, et al. Simultaneous determination of amitraz and its metabolite (2, 4-dimethylaniline) residues in honey by ultra-performance liquid chromatography[J]. Journal of Food Safety & Quality, 2020, 11(12):4091-4096.
[5] 戴雪香, 董霞. 农药对养蜂业的影响[J]. 蜜蜂杂志, 2016, 36(10):12-15.
DAI X X, DONG X. The effects of pesticides on apiculture[J]. Journal of Bee, 2016, 36(10):12-15.
[6] GOULSON D, NICHOLLS E, BOTÍAS C, et al. Bee declines driven by combined stress from parasites, pesticides, and lack of flowers[J]. Science, 2015, 347(6229):1255957.
[7] 黄永舜. 蜂蜜中农药残留的研究进展[J]. 现代食品, 2018(13):66-68.
HUANG Y S. Research progress of pesticide residues in honey[J]. Modern Food, 2018(13):66-68.
[8] KREPPER G, PISTONESI M F, DI NEZIO M S. Adsorptive square wave voltammetric determination of amitraz in Argentine honeys with a microwave-assisted sample treatment[J]. Microchemical Journal, 2019, 150:104068.
[9] BOMMURAJ V, BIRENBOIM M, CHEN Y, et al. Depletion kinetics and concentration- and time-dependent toxicity of a tertiary mixture of amitraz and its major hydrolysis products in honeybees[J]. Chemosphere, 2021, 272:129923.
[10] AMOLI J S, HASAN J, HEJAZY M. Determination of amitraz residue by headspace gas chromatography in honey and beeswax samples from Iran[J]. American Journal of Food Technology, 2008, 4(1):56-59.
[11] 杨媛, 石磊, 张开春, 等. 固相萃取-高效液相色谱法测定水果中单甲脒的残留量[J]. 分析化学, 2010, 38(9):1342-1344.
YANG Y, SHI L, ZHANG K C, et al. Determination of semiamitraz residue in fruits by solid phase extraction-high performance liquid chromatography[J]. Chinese Journal of Analytical Chemistry, 2010, 38(9):1342-1344.
[12] TOKMAN N, SOLER C, LA FARRÉ M, et al. Determination of amitraz and its transformation products in pears by ethyl acetate extraction and liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography. A, 2009, 1216(15):3138-3146.
[13] FUENTE-BALLESTEROS A, BRUGNEROTTO P, COSTA A C O, et al. Determination of acaricides in honeys from different botanical origins by gas chromatography-mass spectrometry[J]. Food Chemistry, 2023, 408:135245.
[14] 谭亚军, 赵甲慧, 李伟, 等. 柑橘类水果中双甲脒及其代谢物的QuEChERS-GC/MS测定法[J]. 职业与健康, 2022, 38(17):2328-2332.
TAN Y J, ZHAO J H, LI W, et al. Determination of amitraz and its metabolites in citrus fruits by QuEChERS-GC/MS[J]. Occupation and Health, 2022, 38(17):2328-2332.
[15] 黄娟, 桂茜雯, 高玲, 等. 高效液相色谱-串联质谱法测定蔬菜水果中双甲脒及其代谢产物[J]. 色谱, 2019, 37(1):1-7.
HUANG J, GUI Q W, GAO L, et al. Determination of amitraz and its metabolites in vegetables and fruits by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2019, 37(1):1-7.
[16] 侯建波, 谢文, 曾淦宁, 等. 液相色谱-串联质谱法测定蜂王浆中双甲脒及其代谢物的残留量[J]. 质谱学报, 2019, 40(2):131-138.
HOU J B, XIE W, ZENG G N, et al. Simultaneous determination of amitraz and its metabolites in royal jelly by HPLC-MS/MS[J]. Journal of Chinese Mass Spectrometry Society, 2019, 40(2):131-138.
[17] 智军海, 孟超, 周嘉明. 双甲脒胶体金免疫快速检测试纸条研制及其在蜂蜜中的应用[J]. 食品安全质量检测学报, 2022, 13(10):3290-3295.
ZHI J H, MENG C, ZHOU J M. Development of amitraz colloidal gold rapid immunoassay strip and its application in honey[J]. Journal of Food Safety & Quality, 2022, 13(10):3290-3295.
[18] WANG F Q, LI S H, FENG H, et al. An enhanced sensitivity and cleanup strategy for the nontargeted screening and targeted determination of pesticides in tea using modified dispersive solid-phase extraction and cold-induced acetonitrile aqueous two-phase systems coupled with liquid chromatography-high resolution mass spectrometry[J]. Food Chemistry, 2019, 275:530-538.