Determination of Glyphosate, Ammonium Phosphate and Ammonia in Tea by UHPLC-MS

doi:10.11924/j.issn.1000-6850.casb20190900621

Abstract

Abstract:

A method is developed for the determination of glufosinate-ammonium (GLUF), glyphosate (PMG) and aminomethylphosphonic acid (AMPA) in tea using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample is extracted with ultrapure water and dichloromethane under ultrasonication, followed by a simple cleanup with a C18 solid phase extraction (SPE) cartridge, and then GLUF, PMG and AMPA are derivatized using 9-fluorenylmethoxycarbonyl (FMOC-Cl) in borate buffer. The derivatives of GLUF, PMG and AMPA are separated on a Waters HSS T3 column 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 is performed by external standard method. The method shows a good linearity (R²>0.999) in the range of 0-100 ng/mL. The limit of detection (LODs) of GLUF, PMG and AMPA is 0.7 g/kg. At the spiked level of 2.0, 4.0和10.0 μg/kg, the recovery of GLUF, PMG and AMPA is 86.3%-100.2%,85.7%-101.5%, and 88.1%-98.4%, respectively, and the relative standard deviation (RSDs) (n=6) of GLUF, PMG and AMPA is 1.1%-5.0% respectively. This method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements for the analysis of GLUF, PMG and AMPA simultaneously in tea.

Key words: UHPLC-MS, glyphosate, glufosinate-ammonium, aminomethylphosphonic acid, tea

CLC Number:

O658

Liu Wenjing, Lin Jing, Fu Jianwei, Wu Jianhong. Determination of Glyphosate, Ammonium Phosphate and Ammonia in Tea by UHPLC-MS[J]. Chinese Agricultural Science Bulletin, 2020, 36(25): 129-136.

Figures/Tables 9

References 25

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化合物	保留时间/min	母离子(m/z)	子离子(m/z)	去簇电压/V	碰撞能量/eV
草甘膦	3.74	392.1	170^*,214	27,27	28,14
草铵膦	3.97	404	136^*,179	30,27	29,16
氨甲基膦酸	3.83	334	112^*,156	22,30	24,19
草甘膦内标	3.74	393.5	179.32^*,214.86	25,25	9,10

化合物	保留时间/min	母离子(m/z)	子离子(m/z)	去簇电压/V	碰撞能量/eV
草甘膦	3.74	392.1	170^*,214	27,27	28,14
草铵膦	3.97	404	136^*,179	30,27	29,16
氨甲基膦酸	3.83	334	112^*,156	22,30	24,19
草甘膦内标	3.74	393.5	179.32^*,214.86	25,25	9,10

分析物	回归方程	线性范围/(ng/mL)	相关系数(r²)	检出限/(μg/kg)	定量限/(μg/kg)
草甘膦	y=420.7x+39.7	1~100	0.9993	0.7	2.0
草铵膦	y=909.4x-67.6	1~100	0.9995	0.7	2.0
氨甲基膦酸	y=1595.7x-52.8	1~100	0.9991	0.7	2.0

分析物	回归方程	线性范围/(ng/mL)	相关系数(r²)	检出限/(μg/kg)	定量限/(μg/kg)
草甘膦	y=420.7x+39.7	1~100	0.9993	0.7	2.0
草铵膦	y=909.4x-67.6	1~100	0.9995	0.7	2.0
氨甲基膦酸	y=1595.7x-52.8	1~100	0.9991	0.7	2.0