Citation: WU Xiaogang, CHEN Xiaoquan, XIAO Haijun, LIU Binqiu. Simultaneous determination of glyphosate and glufosinate- ammonium residues in tea by ultra performance liquid chromatography-tandem mass spectrometry coupled with pre-column derivatization[J]. Chinese Journal of Chromatography, ;2015, 33(10): 1090-1096. doi: 10.3724/SP.J.1123.2015.04045 shu

Simultaneous determination of glyphosate and glufosinate- ammonium residues in tea by ultra performance liquid chromatography-tandem mass spectrometry coupled with pre-column derivatization

1.
Technology Center Laboratory of Menghai Tea Industry Co., Ltd., TAETEA Group, Menghai 666200, China

Corresponding author: WU Xiaogang,
Received Date: 24 April 2015

Fund Project: 云南省企业技术中心创新能力建设项目(2009D1037). (2009D1037)

A method was developed for the determination of glyphosate (GLY) and glufosinate-ammonium (GLUF) in tea using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted with ultrapure water and dichloromethane for 30 min under ultrasonication, followed by a simple cleanup with a C₁₈ solid phase extraction (SPE) cartridge, and then GLY and GLUF were derivatized using 9-fluorenylmethoxycarbonyl (FMOC-Cl) in borate buffer for 2 h. The derivatives of GLY and GLUF were separated on a Waters C₁₈ column (50 mm×2.1 mm, 1.7 μm) in a gradient elution mode, and finally detected with positive electrospray ionization-mass spectrometry (ESI-MS/MS) in multiple reaction monitoring (MRM) mode. The quantification analysis was performed by external standard method. The method showed a good linearity (r> 0.990) in the range of 0.003125-0.1 mg/L. The limits of detection (LODs) of GLY and GLUF were 0.03 mg/kg. At the spiked levels of 0.375, 1.5 and 4.5 mg/kg, the recoveries of GLY and GLUF were 87.37%-99.11% and 81.44%-86.17% respectively, and the relative standard deviations (RSDs) (n=6) of GLY and GLUF were 0.68%-1.35% and 1.01%-2.33%, respectively. This method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements for the analysis of GLY and GLUF simultaneously in tea.
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沈阳化工大学材料科学与工程学院沈阳 110142