摘要
本研究建立了一种稀释同位素内标法测定花生和南瓜籽中三乙膦酸铝及其降解产物乙基膦酸和亚磷酸残留量的检测方法。样品经酸化甲醇提取,冷冻离心,C18吸附剂材料净化,采用Hypercarb色谱柱分离,液相色谱串联质谱仪检测,稀释同位素内标法定量。乙基膦酸和亚磷酸在6.25~250 ng/mL的浓度范围内,线性方程的系数R2>0.999,乙基膦酸和亚磷酸的检出限均为0.05 mg/kg;在0.05 mg/kg、0.15 mg/kg和0.50 mg/kg 3个梯度不同浓度加标水平下,花生和南瓜籽中乙基膦酸和亚磷酸的回收率为88%~106%,6次试验结果的相对标准偏差在8.5%~12.0%之间。该方法样品前处理简便、耗时短,检测耗材成本低、结果准确、稳定性佳,能够满足花生和南瓜籽中三乙膦酸铝及其分解产物乙基膦酸和亚磷酸的残留量的检测要求。
An isotope internal standard method was established to determine residues of fosety-aluminum and its decomposition products,ethylphosphoric acid and phosphonic acid,in peanuts and pumpkin seeds.The samples were extracted with acidified methanol,frozen centrifuged,and purified with C18.Separation was achieved using a Hypercarb chromatographic column,and detection was performed with liquid chromatography-tandem mass spectrometry(LC-MS/MS),followed by quantification using the dilution isotope internal standard method.In the concentration range of 6.25-250 ng/mL for ethylphosphoric acid and phosphonic acid,the linear equations had coefficients(R2)greater than 0.999.The detection limits for ethylphosphoric acid and phosphonic acid were both 0.05 mg/kg.At three different levels of 0.05 mg/kg,0.15 mg/kg,and 0.50 mg/kg,the recoveries of ethylphosphoric acid and phosphonic acid in peanuts and pumpkin seeds ranged from 88%to 106%,and the relative standard deviations of the results from six experiments were between 8.5%and 12.0%.This method has the advantages of simple sample pre-treatment,short analysis time,low consumable cost,accurate results and good stability.It can meet the requirements for the determination of residues of fosety-aluminum and its decomposition products,ethylphosphoric acid and phosphonic acid,in peanuts and pumpkin seeds.
作者
郭雨
施亚申
吉如娜
GUO Yu;SHI Ya-Shen;JI Ru-Na(Alex Stewart Agricultural Ltd,Suzhou215332;Comprehensive Technology Center of Suzhou Customs,Suzhou215104)
出处
《中国口岸科学技术》
2023年第11期63-67,共5页
China Port Science and Technology
关键词
稀释同位素内标
三乙膦酸铝
乙基膦酸
亚磷酸
diluted isotope internal standard
fosety-aluminum
ethylphosphoric acid
phosphonic acid
