Determination of tetraniliprole residues in animal derived foods by multi-plug filtration cleanup combined with HPLC-MS/MS

Authors

YUAN Liejiang, Hunan Provincial Institute of Product and Goods Quality Inspection , Changsha , Hunan 410007 , China;Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning , Changsha , Hunan 410111 , China
WANG Xiu, Hunan Provincial Institute of Product and Goods Quality Inspection , Changsha , Hunan 410007 , China;Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning , Changsha , Hunan 410111 , China
LI Zheng, Hunan Provincial Institute of Product and Goods Quality Inspection , Changsha , Hunan 410007 , China;Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning , Changsha , Hunan 410111 , China
ZHU Li, Hunan Provincial Institute of Product and Goods Quality Inspection , Changsha , Hunan 410007 , China;Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning , Changsha , Hunan 410111 , China;Yueyang Inspection and Testing Center , Yueyang , Hunan 410042 , ChinaFollow
DENG Hang, Hunan Provincial Institute of Product and Goods Quality Inspection , Changsha , Hunan 410007 , China;Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning , Changsha , Hunan 410111 , China

Corresponding Author(s)

朱礼（1983—），女，岳阳市检验检测中心高级工程师，硕士。E-mail：251866823@qq.com

Abstract

［［Objective ］］ This study aimed to develop a rapid and efficient method for quantifying tetraniliprole residues in animal -derived foods by combining multi -plug filtration cleanup (m-PFC ) with high -performance liquid chromatography -mass spectrometry (HPLC -MS).［［Methods ］］ Samples were extracted with acetonitrile,followed by salting out using sodium chloride and anhydrous magnesium sulfate.The extracts were purified via m -PFC and analyzed using HPLC -MS with external standard calibration.［［Results］］ The method demonstrated a strong linear correlation between tetraniliprole concentration and response values over a range of 0.001 to 0.150 mg/L,with a coefficient of determination (R2) exceeding 0.999.The limit of quantification (LOQ ) was 0.002 mg/kg.Average recovery rates ranged from 90.0% to 108.0%,with relative standard deviations between 1.10% and 4.89%,validated across a variety of matrices,including pork,beef,mutton,chicken,pork liver,beef liver,mutton liver,chicken liver,eggs and milk.［［Conclusion ］］ The proposed method is rapid,straightforward,high sensitivity,and suitable for quantitative determination of tetraniliprole residues in animal -derived food.

Publication Date

2-18-2025

First Page

46

Last Page

52

DOI

10.13652/j.spjx.1003.5788.2024.80800

Recommended Citation

Liejiang, YUAN; Xiu, WANG; Zheng, LI; Li, ZHU; and Hang, DENG (2025) "Determination of tetraniliprole residues in animal derived foods by multi-plug filtration cleanup combined with HPLC-MS/MS," Food and Machinery: Vol. 40: Iss. 10, Article 7.
DOI: 10.13652/j.spjx.1003.5788.2024.80800
Available at: https://www.ifoodmm.cn/journal/vol40/iss10/7

References

[1] 杨吉春,吴峤,王秀丽.2014年公开的新农药品种 [J].农药,2015,54(3):215-216,226.YANG J C,WU Q,WANG X L.New pesticide varieties opened in 2014 [J].Pesticide,2015,54(3):215-216,226.
[2] 徐勋鹏.杀虫剂四唑虫酰胺的合成 [D].武汉:武汉工程大学,2023.XU X P.Synthesis of insecticide tetraniliprole [D].Wuhan:Wuhan Institute of Technology,2023.
[3] 盛祝波,汪杰,裴鸿艳,等.新型杀虫剂四唑虫酰胺 [J].农药,2021,60(1):52-56,60.SHENG Z B,WANG J,PEI H Y,et al.New insecticide tetraniliprole [J].Pesticide,2021,60(1):52-56,60.
[4] 池艳艳,林少源,陈炳旭,等.四唑虫酰胺对草地贪夜蛾的毒力评价及田间防效 [J].中国农学通报,2023,39(7):111-115.CHI Y Y,LIN S Y,CEHN B X,et al.Toxicity evaluation and field control effect of tetrazolamide on Armyworm of grassland[J].Chinese Agricultural Science Bulletin,2023,39(7):111-115.
[5] 张静,武鹏,陈立萍,等.四唑虫酰胺种子处理悬浮剂高效液相色谱分析方法研究 [J].农药科学与管理,2017,38(5):48-51.ZHANG J,WU P,CHEN L P,et al.Study on HPLC method of tetrazolamide seed treatment suspension [J].Pesticide Science and Management,2017,38(5):48-51.
[6] 李卫,张月,贾浩然,等.18%四唑虫酰胺悬浮剂高效液相色谱分析方法 [J].现代农药,2019,18(4):32-34.LI W,ZHANG Y,JIA H R,et al.Method for analysis of 18% tetrazolamide suspension by high performance liquid chromatography [J].Modern Pesticide,2019,18(4):32-34.
[7] 李卫,张月,贾浩然,等.18%四唑虫酰胺悬浮剂高效液相色谱串联质谱的分析方法 [J].农药,2019,58(5):344-346.LI W,ZHANG Y,JIA H R,et al.Method for analysis of 18% tetrazolamide suspension by high performance liquid chromatography-tandem mass spectrometry [J].Pesticide,2019,58(5):344-346.
[8] LIM S H,DO J A,PARK S M,et al.Development of the analytical method for insecticide tolfenpyrad determination in agricultural commodities using LC-MS/MS [J].The Korean Journal of Pesticide Science,2018,22(2):143-152.
[9] LI W,ZHANG Y,JIA H R,et al.Residue analysis of tetraniliprole in rice and related environmental samples by HPLC/MS [J].Microchemical Journal,2019,150:104168.
[10] 谢思敏,古锶巧,顾利红,等.mPFC-QuEChERS 净化联合UPLC-MS/MS 法快速测定 3种根茎类中药材中 16种真菌毒素[J].分析测试学报,2024,43(7):1 003-1 010.XIE S M,GU S Q,GU L H,et al.The mPFC-QuEChERS purification combined with UPLC-MS/MS method was used for the rapid determination of 16 mycotoxins in 3 rhizome Chinese medicinal materials [J].Journal of Analysis and Testing,2024,43(7):1 003-1 010.
[11] 马金晶,金玉娥,周婧娴.HPLC-MS/MS 结合液液萃取法检测尿样中 22种新烟碱类农药及其代谢物的研究 [J].分析测试学报,2024,43(8):1 257-1 264.MA J J,JIN Y E,ZHOU J X.Determination of 22 neonicotinoids and their metabolites in urine samples by HPLC-MS/MS combined with liquid-liquid extraction [J].Journal of Analysis and Testing,2024,43(8):1 257-1 264.
[12] 黄柳芳.食品中农药残留检测的样品前处理技术研究 [J].食品安全导刊,2023 (6):142-144.HUANG L F.Study on sample pretreatment technology for detection of pesticide residues in food [J].Food Safety Guide,2023 (6):142-144.
[13] 万娜,潘永波,梁晓涵,等.快速滤过型净化结合超高效液相色谱—串联质谱法同时测定鸡蛋中 38种杀菌剂类农药残留[J].食品工业科技,2023,44(17):324-333.WAN N,PAN Y B,LIANG X H,et al.Rapid filtration purification combined with ultra-high performance liquid chromatography-tandem mass spectrometry for the simultaneous determination of 38 fungicide pesticide residues in eggs [J].Food Industry Science and Technology,2023,44(17):324-333.
[14] 刘松南,田旭,高晶,等.快速滤过型净化结合液相色谱—质谱联用法测定茶叶中特丁硫磷及其 5种代谢产物 [J].食品科学,2022,43(4):284-290.LIU S N,TIAN X,GAO J,et al.Determination of tert-butylthiophosphorus and its 5 metabolites in tea by rapid filtration purification combined with liquid chromatography-mass spectrometry [J].Food Science,2022,43(4):284-290.
[15] 孟志娟,黄云霞,邸鹏月,等.快速滤过型净化法结合气相色谱—四极杆—飞行时间质谱同时筛查果蔬中 234种农药残留[J].食品科学,2020,41(16):272-285.MENG Z J,HUANG Y X,DI P Y,et al.The rapid filtration purification method combined with gas chromatography-quadrupole-time-of-flight mass spectrometry was used to screen 234 pesticide residues in fruits and vegetables [J].Food Science,2020,41(16):272-285.
[16] 潘永波,万娜,王承业,等.快速滤过型净化结合液相色谱—质谱联用法测定海产品中 19种磺胺类药物残留 [J].食品工业科技,2023,44(7):320-328.PAN Y B,WAN N,WANG C Y,et al.Determination of 19 sulfonamides residues in seafood by rapid filtration purification combined with liquid chromatography-mass spectrometry [J].Food Industry Science and Technology,2023,44(7):320-328.
[17] 王小乔,李坚,许晓辉,等.超滤型高脂基质净化柱结合超高效液相色谱—三重四极杆液质联用法测定鱼肉中 7种镇静剂[J].食品与发酵工业,2023,49(24):267-274.WANG X Q,LI J,XU X H,et al.Determination of seven kinds of sedative in fish by MPFC-QuEChERS combined with UPLC-MS/MS [J].Food and Fermentation Industry,2023,49(24):267-274.
[18] 王献礼,饶钦雄,张其才,等.快速滤过型净化结合超高效液相色谱—串联质谱法测定中华绒螯蟹中 14种全氟烷基化合物[J].色谱,2023,41(12):1 095-1 105.WANG X L,RAO Q X,ZAHNG Q C,et al.Determination of 14 perfluoroalkyl compounds in Chinese mitten crab by multri-plug filtration cleanup coupled with ultra-high performance liquid chromatography- tandem mass spectrometry [J].Chromatography,2023,41(12):1 095-1 105.
[19] KITTLAUS S,SCHIMANKE J,KEMPE G,et al.Assessment of sample cleanup and matrix effects in the pesticide residue analysis of foods using postcolumn infusion in liquid chromatography –tandem mass spectrometry [J].Journal of Chromatography A,2011,1 218(46):8 399-8 410.
[20] 贺敏,景子伟,贾春虹,等.超高效液相色谱—串联质谱法检测番茄和甘蓝中溴虫氟苯双酰胺的残留 [J].农药,2019,58(4):279-281,284.HE M,JING Z J,JIA C H,et al.Simultaneous determination of broflanilide residues in tomato and cabbage by UPLC-MS/MS[J].Pesticide,2019,58(4):279-281,284.
[21] 李占彬,赵丽君,黄永桥,等.MPFC-QuECHERS 结合超高效液相色谱串联质谱法快速测定铁皮石斛中 56种农药残留[J].食品与机械,2023,39(7):48-55,84.LI Z B,ZHAO L J,HUANG Y Q,et al.Rapid determination of 56 pesticide residues in Dendrobium officinale by MPFC-QuECHERS method combined with ultra-performance liquid chromatography-tandem mass spectrometry [J].Food & Machinery,2023,39(7):48-55,84.