Determination of glyphosate and aminomethylphosphonic acid in rice using liquid chromatography-tandem mass spectrometry
液相色谱-串联质谱法测定稻米中的草甘膦和氨甲基膦酸残留

A method was developed for the determination of glyphosate (GLY) and amino-methylphosphonic acid (AMPA) in rice using liquid chromatography tandem mass spectrometry (LC-MS/MS). The sample was extracted with water followed by a simple cleanup with a C18 solid phase extraction (SPE) cartridge, and then GLY and AMPA were derivatized using 9-fluorenylmethoxycarbonyl (FMOC-Cl) in borate buffer. The derivatives of GLY and AMPA were separated on a C18 column with gradient elution with the mobile phase of acetonitrile and 5 mmol/L ammonium acetate (pH 9), and finally detected with negative ion electrospray ionization-mass spectrometry (ESI-MS) in multiple reaction monitoring (MRM) mode. The results showed that the linearities of GLY and AMPA were in the concentration range of 0.00050 to 1.0 mg/L with the correlation coefficients of 0.9997 and 0.9999, respectively. The mean spiked recoveries of GLY and AMPA at 3 spiked levels ranged from 72.5% to 113.6% with the relative standard deviations (RSD, n=5) of 3.8%-16.2%. The limits of detection were 2.0 and 3.0 μg/kg for GLY and AMPA, respectively. This method is rapid, sensitive, and suitable for simultaneous determination of GLY and AMPA in rice.