摘要
建立超高效液相色谱-质谱联用法测定羊奶和羊奶粉中安乃近(4-氨基安替比林、4-甲酰氨基安替比林、4-乙酰氨基安替比林和4-甲基氨基安替比林)残留量的分析方法。样品经乙腈提取,氮吹浓缩,以甲酸水和甲酸乙腈作为流动相,通过超高效液相色谱,采用ESI正离子模式多反应监测,4-氨基安替比林、4-甲酰氨基安替比林、4-乙酰氨基安替比林用外标法定量,4-甲基氨基安替比林用同位素内标定量。4-氨基安替比林在0~99.1μg/L范围内,其他3个化合物在0~99.9μg/L范围内的线性关系良好,相关系数R2均大于0.995。4-氨基安替比林、4-甲酰氨基安替比林、4-乙酰氨基安替比林和4-甲基氨基安替比林的定量限分别为2.8,3.9,0.088和1.4μg/kg。当羊奶加标水平约5,10,20和50μg/kg,羊奶粉约40,80,160和400μg/kg时,回收率为83.6%~100.2%,方法的精密度相对标准偏差为0.3%~6.5%(n=6)。该方法灵敏、准确,能够快速、有效检测羊奶和羊奶粉中安乃近残留量,可用于日常风险监测和市场监管。
An analytical method was developed for the determination of metamizole sodium(4-aminoantipyrine,4-formylaminoantipyrine,4-acetamidoantipyrine and 4-methylaminoantipyrine)residues in goat milk and goat milk powder by UPLC-MS/MS.The samples were extracted with acetonitrile,concentrated by nitrogen,and mobile phases were formic acid water and formic acid acetonitrile.The identification and quantification of metamizole sodium residues were carried out by UPLC-MS/MS with multiple reaction monitoring in positive electrospray ionization.4-aminoantipyrine,4-formylaminoantipyrine and 4-acetaminoantipyrine were quantified by external standard method,and 4-methylaminoantipyrine was quantified by isotopic internal standard.The linearity of 4-aminoantipyrine in the range of 0-99.1μg/L and the other three compounds in the range of 0-99.9μg/L was good,with the correlation coefficients(R2)more than 0.995.The limits of quantification of 4-aminoantipyrine,4-formylaminoantipyrine,4-acetylaminoantipyrine,and 4-methylaminoantipyrine were 2.8,3.9,0.088,and 1.4μg/kg,respectively.The recoveries ranged from 83.6%to 100.2%at spiked levels of about 5,10,20 and 50μg/kg for goat milk,and 40,80,160 and 400μg/kg for goat milk powder.The relative standard deviations of the precision was 0.3%-6.5%(n=6).The method was sensitive,accurate,fast and effective for the determination of metamizole sodium residues in goat milk and goat milk powder,which could be used for daily risk monitoring and market supervision.
作者
李璐
杨家秀
王聪
董文君
张艳
LI Lu;YANG Jiaxiu;WANG Cong;DONG Wenjun;ZHANG Yan(Center of Inspection and Research in Fuping(Shaanxi Provincial Goat Milk Product Quality Supervision and Testing Center),Fuping 711700;Shaanxi Shengtang Dairy Co.,Ltd.,Fuping 711700)
出处
《食品工业》
CAS
2024年第2期288-292,共5页
The Food Industry
基金
陕西省市场监督管理局科技计划项目(2022KY22)
渭南市科技计划项目(2022ZDYFJH-47)。
关键词
安乃近
羊奶
羊奶粉
超高效液相色谱-质谱联用(UPLC-MS/MS)
metamizole sodium
goat milk
goat milk powder
ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
