色谱2012，Vol.30Issue(1)：39-44,6.DOI:10.3724/SP.J.1123.2011.08040
亲水作用色谱-串联质谱法测定稻米中的草甘膦和氨甲基磷酸残留量
Determination of glyphosate and aminomethylphosphonic acid in rice using hydrophilic interaction chromatographytandemmass spectrometry
摘要
Abstract
A method was developed for the simultaneous determination of glyphosate (Gly) and aminomethylphosphonic acid (AMPA) residues in rice using hydrophilic interaction chro-matography-tandem mass spectrometry (HILIC-MS/MS). The samples were extracted with water, and purified using a C18 solid phase extraction cartridge followed by an ultrafiltration membrane to remove interfering materials. Gly and AMPA were separated on an HILIC column with the mobile phases of 1 mmol/L ammonium acetate (pH 11.0 adjusted with ammonium hydroxide) and acetonitrile, and finally detected with negative electrospray ionization (ESI") in multiple reaction monitoring (MRM) mode. The matrix-matched external standard calibration curves were used for quantitative analysis. The sample pretreatment of Gly and its metabolite was successfully carried out without any derivatization. Under the optimal analytical conditions, the linearities of Gly and AMPA were in the concentration ranges of 0. 001 to 0. 250 mg/L and 0. 002 5 to 0. 250 mg/L respectively, with the correlation coefficients of 0. 999 5 for the both analytes. The limits of detection (S/N = 3) of the method were 0.010 mg/kg for Gly, and 0.020 mg/kg for AMPA. For all the samples, the mean spiked recoveries of Gly and AMPA were in the range from 96. 3% to 107. 3% at 3 spiked levels (0. 100, 0. 500 and 2. 500 mg/kg), and the relative standard deviations (RSDs, n =3) were in the range of 1. 3% -9. 1%. The method is easy, fast, sensitive and accurate, and can meet the requirements of the determination of Gly and AMPA pesticide residues in rice.关键词
亲水作用色谱-串联质谱/草甘膦/氨甲基磷酸/稻米Key words
hydrophilic interaction chromatography-tandem mass spectrometry (HILIC-MS/ MS) / glyphosate/ aminomethylphosphonic acid/ rice分类
化学化工引用本文复制引用
江燕,曹赵云,贾瑞琳,齐慧,陈铭学..亲水作用色谱-串联质谱法测定稻米中的草甘膦和氨甲基磷酸残留量[J].色谱,2012,30(1):39-44,6.基金项目
中央级公益性科研院所基本科研业务费专项资金项目(2009 RG006)和农业行业标准制定资金项目(2004-62). （2009 RG006）
