乳业科学与技术2025，Vol.48Issue(3)：43-48,6.DOI:10.7506/rykxyjs1671-5187-20241223-112
超高效液相色谱-串联质谱法测定牛乳中乙烯利残留
Determination of Ethephon Residue in Milk by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method with solid phase extraction(SPE)was established for the detection of ethephon residue in milk.In the sample pretreatment stage,formic acid solution was selected as the extraction solvent,and the extract was purified on an amino SPE column.The target compound was separated on a Waters Anionic Polar Pesticide column(150 mm×2.1 mm,5 μm)using gradient elution with a mobile phase consisting of 0.1%formic acid containing 50 mmol/L ammonium formate and acetonitrile.The detection was performed using electrospray ionization in the negative ion mode with multiple reaction monitoring,and the matrix-matched external standard method was used for quantification.The calibration curve for ethephon showed an excellent linearity(r2>0.99)in the concentration range of 2 to 100 ng/mL,and the limit of detection and limit of quantification of this method were 0.5 and 1.0 μg/kg,respectively.At spiked concentration levels of 1.0,2.0 and 10.0 μg/kg,the recoveries were between 92.50%and 113.76%,and the precision,expressed as relative standard deviation,ranged from 3.04%to 4.60%.In conclusion,the UPLC-MS/MS method has the advantages of high accuracy,specificity,and repeatability,and is very suitable for the determination of ethphon in milk.关键词
超高效液相色谱-串联质谱法/牛乳/乙烯利/固相萃取Key words
ultra-high performance liquid chromatography-tandem mass spectrometry/milk/ethephon/solid phase extraction分类
轻工纺织引用本文复制引用
白艳梅,张立佳,汪洋,刘丽君,莫楠,高玉杰,李培珍,胡雪,吴晓莉..超高效液相色谱-串联质谱法测定牛乳中乙烯利残留[J].乳业科学与技术,2025,48(3):43-48,6.基金项目
国家市场监督管理总局重点实验室项目(991100000380) （991100000380）
