Glyphosate and Aminomethyl Phosphonic Acid in Soil: Determined by Direct Injection Liquid Chromatography-tandem Mass Spectrometry

doi:10.11924/j.issn.1000-6850.casb20200300285

Abstract

Abstract:

In order to establish a quantitative analysis method for glyphosate and its major metabolite aminomethyl phosphonic acid (AMPA) residues in soil, the solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry technology was used in this study. The sample was extracted with sodium sulfate and trisodium citrate, purified by solid phase extraction, isolated by hydrophilic liquid chromatographic column, detected by chromatography-tandem mass spectrometry under negative electro-spray ionization in the multiple reaction monitoring mode (MRM) and quantified by the external standard method. The results showed that the good linearity range of glyphosate and AMPA was 0.02-2 μg/mL, their correlation coefficients (R²) were 0.9995 and 0.9998. The limit of detection (LOD) of glyphosate and AMPA was 0.5 μg/kg and 0.6 μg/kg, respectively, and the limit of quantification (LOQ) was1.6 μg/kg and 2.0 μg/kg, respectively. The recovery of glyphosate and AMPA at three spiked concentration levels ranged from 79.67% to 96.17% and from 77.83% to 99.47%, respectively. RSD was 3.95%-7.49% and 1.96%-3.89%, respectively. Compared with the traditional derivatization method, this method has the advantages such as the simple operation, low LOD and high accuracy, and it is suitable for analyzing glyphosate and aminomethyl phosphonic acid in soil.

Key words: soil, glyphosate, aminomethyl phosphonic acid, solid phase extraction, ultra high performance liquid chromatography-mass spectrometry

CLC Number:

Zhou Qin, Wu Yumei. Glyphosate and Aminomethyl Phosphonic Acid in Soil: Determined by Direct Injection Liquid Chromatography-tandem Mass Spectrometry[J]. Chinese Agricultural Science Bulletin, 2020, 36(27): 72-80.

Figures/Tables 10

References 26

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步骤	分析时间/min	流速/(μL/min)	A/%	B/%
1	0	250	90	10
2	0.5	250	90	10
3	3.5	250	10	90
4	6.5	250	10	90
5	6.6	250	90	10
6	8.00	250	90	10

步骤	分析时间/min	流速/(μL/min)	A/%	B/%
1	0	250	90	10
2	0.5	250	90	10
3	3.5	250	10	90
4	6.5	250	10	90
5	6.6	250	90	10
6	8.00	250	90	10

名称	Q1 (Da)	Q3 (Da)	Time (mses)	去簇电压（DP） (volts)	入口电压（EP） (volts)	碰撞能量（CE） (volts)	出口电压（CXP） (volts)
草甘膦（Glyphosate 1）	390.0	150.0	50	-60	-10	-25	-7
草甘膦（Glyphosate 2）	390.0	168.0	50	-65	-10	-16	-13
氨甲基膦酸（AMPA 1）	332.0	136.0	50	-15	-10	-16	-15
氨甲基膦酸（AMPA 2）	332.0	110.0	50	-15	-10	-8	-13

名称	Q1 (Da)	Q3 (Da)	Time (mses)	去簇电压（DP） (volts)	入口电压（EP） (volts)	碰撞能量（CE） (volts)	出口电压（CXP） (volts)
草甘膦（Glyphosate 1）	390.0	150.0	50	-60	-10	-25	-7
草甘膦（Glyphosate 2）	390.0	168.0	50	-65	-10	-16	-13
氨甲基膦酸（AMPA 1）	332.0	136.0	50	-15	-10	-16	-15
氨甲基膦酸（AMPA 2）	332.0	110.0	50	-15	-10	-8	-13

样品	农药名称	样本数	加标水平/(mg/g)	测定值/(mg/g)	平均回收率/%	RSD/%
土壤	草甘膦	6	0.05	0.037~0.043	79.67	5.82
			1.00	0.78~0.89	82.67	3.95
			5.00	4.46~5.21	96.17	7.49
	氨甲基膦酸	6	0.1	0.076~0.081	77.83	2.75
			2.00	1.79~2.01	94.25	3.89
			6.00	96.0~100.7	99.47	1.96