Abstract
［Objective］ To establish an analytical method for the determination of residues of eight fungicides ametoctradin, triadimefon,triadimenol, flutriafol, mandipropamid, penthiopyrad, isopyrazam, and prochloraz ) in eggs by solid -phase extraction (SPE) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS ).［Methods］ The samples are ultrasonically extracted with acetonitrile. The extracts are purified using ProElut DPC solid -phase extraction cartridges. The purified eluate is concentrated under reduced pressure and reconstituted with acetonitrile.Chromatographic separation is performed on a Kinetex C18 column (2.6 μm,2.1 mm ×100 mm ) with gradient elution using 0.1% formic acid in water and acetonitrile as the mobile phase. Detection is carried out using electrospray ionization (ESI) in positive ion mode with multiple reaction monitoring (MRM ),and quantification is performed using the external standard method.［Results］ The eight fungicides exhibit good linearity within their respective concentration ranges (R2>0.99).The limits of detection (LODs ) range from 0.03 to 0.50 μg/kg,and the limits of quantification (LOQs ) range from 0.10 to 2.00 μg/kg. The average recoveries range from 81.6% to 107.0%.［Conclusion］ The established method is simple, accurate, and reproducible, making it suitable for the determination of fungicide residues in eggs.
Publication Date
6-17-2026
First Page
77
Last Page
83
DOI
10.13652/j.spjx.1003.5788.2026.60063
Recommended Citation
Jun, LIANG; Xiong, CHEN; Yu, WANG; Zihao, QU; Wei, ZHANG; and Qing, LI
(2026)
"Determination of eight fungicide residues in eggs by solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry,"
Food and Machinery: Vol. 42:
Iss.
5, Article 9.
DOI: 10.13652/j.spjx.1003.5788.2026.60063
Available at:
https://www.ifoodmm.cn/journal/vol42/iss5/9
References
[1] 秦晓彤,王东,赵尔成,等.基于 UPLC-MS/MS 技术的黄瓜中吡噻菌胺和氟菌唑残留特征解析与风险评估 [J].食品科学,2025,46(19):265-272.QIN X T,WANG D,ZHAO E C,et al.Residue characteristics and health risk assessment of penthiopyrad and triflumizole in cucumber using UPLC-MS/MS [J].Food Science,2025,46(19):265-272.
[2] MAO J C,WU X D,LUO F M,et al.Determination of 19 succinate dehydrogenase inhibitor fungicides pesticide residues in green coffee by quechers-liquid chromatography tandem mass spectrometry [J].Science & Technology of Cereals,Oils & Foods,2023,31(3):159-167.
[3] 岑建斌,罗先勇,李吉龙,等.固相萃取—高效液相色谱—串联质谱法同时测定水果中 9种琥珀酸脱氢酶杀菌剂 [J].分析科学学报,2025,41(3):299-306.CEN J B,LUO X Y,LI J L,et al.Simultaneous determination of nine succinate dehydrogenase fungicides in fruits by solid phase extraction and high performance liquid chromatography-tandem mass spectrometry [J].Journal of Analytical Science,2025,41(3):299-306.
[4] MASÍS-MORA M,BEITA-SANDÍ W,RODRÍGUEZ-YÁÑEZ J,et al.Validation of a methodology by LC-MS/MS for the determination of triazine,triazole and organophosphate pesticide residues in biopurification systems [J].Journal of Chromatography B:Analytical Technologies in the Biomedical and Life Sciences,2020,1 156:122296.
[5] SUN Q R,HUANG Y K,LIU J,et al.Method development,residue level analysis,and dietary risk assessment of 25 novel pesticide residues in animal-derived foods based on modified QuEChERS-HPLC-MS/MS [J].Microchemical Journal,2025,208(1):112586.
[6] 罗景阳,王岩松,李巧莲,等.QuEChERS- 超高效液相色谱—三重四极杆复合线性离子阱质谱法测定鸡蛋中 34种新型杀虫剂的残留量 [J].理化检验:化学分册,2025,61(9):1 101-1 109.LUO J Y,WANG Y S,LI Q L,et al.Determination of residues of 34 novel insecticides in eggs by ultra-high performance liquid chromatography-triple quadrupole composite linear ion trap mass spectrometry with QuEChERS [J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2025,61(9):1 101-1 109.
[7] 袁帅,罗景阳,宋健,等.QuEChERS- 液相色谱串联高分辨质谱法同时测定鸡蛋中 34种杀虫剂的农药残留 [J].食品科技,2025,50(8):326-333.YUAN S,LUO J Y,SONG J,et al.Simultaneous detection of 34 pesticides residues in eggs by QuEChERS-liquid chromatography tandem high resolution mass spectrometry [J].Food Science and Technology,2025,50(8):326-333.
[8] 唐俗,卓程梆,朱雨田,等.高效液相色谱—串联质谱法测定鸡蛋中 18种拟除虫菊酯类农药残留 [J].粮食与油脂,2025,38(1):157-162.TANG S,ZHUO C B,ZHU Y T,et al.Determination of 18 pyrethroid pesticide residues in eggs by high performance liquid chromatography tandem mass spectrometry [J].Cereals & Oils,2025,38(1):157-162.
[9] QIAN J R,ZHANG Y F,LI X W,et al.Determination of four pesticide residues in pepper oleoresin and pepper essential oil using GPC-QuEChERS-GC-MS/MS and dietary risk assessment[J].Journal of chinese mass spectrometry society,2025,46(2):233-241.|[10] 李敏青,陈姿竹,李菊,等.QuEChERS- 高效液相色谱—串联质谱法同时测定动物源性食品中 21种琥珀酸脱氢酶抑制剂类杀菌剂的残留量 [J].分析科学学报,2024,40(5):501-510.LI M Q,CHEN Z Z,LI J,et al.QuEChERS-high performance liquid chromatography-tandem mass spectrometry for determination of 21 succinate dehydrogenase inhibitor fungicides in animal foods [J].Journal of Analytical Science,2024,40(5):501-510.
[11] HOU X G,HOU Z G,WEI L P,et al.Simultaneous determination of multiple pyrazole amide fungicide residues in 12 foodstuffs by QuEChERS-HPLC-MS/MS [J].Journal of Food Composition and Analysis,2025,148(11):108182.
[12] 李巧莲,罗景阳,张宏宏,等.多壁碳纳米管改进 QuEChERS-液相色谱—串联质谱法测定豆类中 12种酰胺类杀菌剂残留量[J].粮食与油脂,2023,36(1):157-162.LI Q L,LUO J Y,ZHANG H H,et al.Determination of 12 amide fungicides in legumes by multi-walled carbon nanotubes QuEChERS-liquid chromatography-tandem mass spectrometry [J].Cereals & Oils,2023,36(1):157-162.
[13] 沈霞.分散固相萃取 /超高效液相色谱—串联质谱法测定食用菌中 19种杀虫剂、杀菌剂及其代谢物 [J].分析测试学报,2020,39(9):1 105-1 111.SHEN X.Determination of 19 insecticides,fungicides and their metabolites in edible fungi by ultra performance liquid chromatography-tandem mass spectrometry with dispersed solid phase extraction [J].Journal of Instrumental Analysis,2020,39(9):1 105-1 111.
[14] 黄彪,刘文静,吴建鸿.分散固相萃取法结合 UPLC-MS/MS同时分析茶叶中 13种杀菌剂 [J].福建茶叶,2019,41(5):13-15.HUANG B,LIU W J,WU J H.Simultaneous analysis of 13 fungicides in tea leaves by dispersive solid-phase extraction combined with UPLC-MS/MS [J].Tea in Fujian,2019,41(5):13-15.
[15] 刘瑾,李利,李莉,等.乳化液液微萃取—超高效液相色谱—串联质谱法检测食品中的三唑类杀菌剂 [J].分析试验室,2024,43(8):1 094-1 101.LIU J,LI L,LI L,et al.Emulsive liquid-liquid microextraction-ultra-high performance liquid chromatography- tandem mass spectrometry for detecting triazole fungicides in food [J].Chinese Journal of Analysis Laboratory,2024,43(8):1 094-1 101.
[16] 康琬琳,张艳超,宋惜木,等.抽拔辅助分散固相微萃取技术用于饮料中 5种杀菌剂残留检测研究 [J].农药学学报,2023,25(6):1 340-1 348.KANG W L,ZHANG Y C,SONG X M,et al.Employing syringe-assisted dispersive solid phase microextraction for precision detection of five fungicide residues in beverages [J].Chinese Journal of Pesticide Science,2023,25(6):1 340-1 348.
[17] 罗宽能,黄子杰,黄朋勉,等.Sin-QuEChERS Nano-UPLC-MS/MS检测大米中甲氨基阿维菌素苯甲酸盐残留 [J].食品与机械,2025,41(8):61-65.LUO K N,HUANG Z J,HUANG P M,et al.Determination of residual emamectin benzoate in rice by Sin-QuEChERS Nano-UPLC-MS/MS [J].Food & Machinery,2025,41(8):61-65.
[18] KEKLIK M,GOLGE O,GONZALEZ-CURBELO M A,et al.Determination of pesticide residues in vine leaves using the QuEChERS method and liquid chromatography-tandem mass spectrometry [J].Foods,2024,13(6):909.
[19] 康绍英,李灿,赵红清,等.高效液相色谱—三重四极杆质谱法测定酒类产品中 59种非法添加药物 [J].食品与机械,2025,41(1):86-96.KANG S Y,LI C,ZHAO H Q,et al.Determination of 59 illegal drugs in alcoholic products by high performance liquid chromatography-triple quadrupole mass spectrometry [J].Food & Machinery,2025,41(1):86-96.
[20] 徐曼,宋少龙,胡俊,等.QuEChERS 结合超高效液相色谱—串联质谱法测定新疆馕制品中丙烯酰胺 [J].食品与机械,2024,40(11):61-68.XU M,SONG S L,HU J,et al.QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry to determine acrylamide in Xinjiang Naan products [J].Food & Machinery,2024,40(11):61-68.
[21] 朱礼,邓航,袁列江,等.QuEChERS 净化结合超高效液相色谱串联质谱法快速测定动物源性食品中溴虫氟苯双酰胺残留[J].食品与发酵工业,2024,50(17):336-342.ZHU L,DENG H,YUAN L J,et al.Rapid determination of broflanilide residues in animal-derived foods by QuEChERS purification combined with UPLC-MS/MS [J].Food and Fermentation Industries,2024,50(17):336-342.
[22] UCLÉS S,LOZANO A,SOSA A,et al.Matrix interference evaluation employing GC and LC coupled to triple quadrupole tandem mass spectrometry [J].Talanta,2017,174:72-81.
[23] LY T K,HO T D,BEHRA P,et al.Determination of 400 pesticide residues in green tea leaves by UPLC-MS/MS and GC-MS/MS combined with QuEChERS extraction and mixed-mode SPE cleanup method [J].Food Chemistry,2020,326:126928.
