Determination of Six Types of Phenoxy Acid Herbicides in Water by Gas Chromatography-Mass Spectrometry with Liquid-Liquid Extraction and Derivatization

doi:10.11924/j.issn.1000-6850.casb2024-0737

Abstract

Abstract:

A method for determination of 6 phenoxy acid herbicides in water by gas chromatography-mass spectrometry was established. After liquid-liquid extraction with dichloromethane, the extract was dehydrated and concentrated, then derivatized with PFBBR under the catalysis of potassium carbonate. The derivatives were analyzed by gas chromatography-mass spectrometry. Samples were separated by Rtx-5ms capillary chromatography column, detected by SIM mode, and quantified by internal standard. The results showed that under the optimal experimental conditions, 6 phenoxy acid herbicides showed good linear relationships in the concentration range of 0.5 to 20.0 μg/mL, the correlation coefficient was not less than 0.999. The detection limit was 0.2 μg/L, and the precision range was 2.2%-6.9%. The spiked tests were conducted on groundwater, surface water, seawater, domestic sewage, and industrial wastewater samples, and the recovery range was 83.0%-113%. Results showed that this method had good precision and stable recovery, providing an effective solution for the detection of phenoxy acid herbicides in water.

Key words: liquid-liquid extraction, derivatization, gas chromatography-mass spectrometry, phenoxy acid herbicides, analysis method

WANG Yuanyuan, LIANG Jing, WANG Lingling, LAI Xiaoshan. Determination of Six Types of Phenoxy Acid Herbicides in Water by Gas Chromatography-Mass Spectrometry with Liquid-Liquid Extraction and Derivatization[J]. Chinese Agricultural Science Bulletin, 2025, 41(11): 159-164.

Figures/Tables 8

References 26

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水平	因素
水平	衍生剂用量/µL	催化剂用量/µL	反应温度/℃	反应时间/h
1	100	10	室温	2
2	200	20	40	3
3	300	30	60	4

水平	因素
水平	衍生剂用量/µL	催化剂用量/µL	反应温度/℃	反应时间/h
1	100	10	室温	2
2	200	20	40	3
3	300	30	60	4

试验号	衍生剂用量/µL	催化剂用量/µL	反应温度/℃	反应时间/h	6种苯氧羧酸类除草剂回收率之和
1	100	10	室温	2	2.151
2	100	20	40	3	4.495
3	100	30	60	4	4.134
4	200	10	40	4	4.476
5	200	20	60	2	3.610
6	200	30	室温	3	2.877
7	300	10	60	3	4.879
8	300	20	室温	4	3.390
9	300	30	40	2	5.426
均值1	3.593	3.835	2.806	3.729
均值2	3.654	3.832	4.799	4.084
均值3	4.565	4.146	4.208	4.000
极差	0.972	0.314	1.993	0.355

试验号	衍生剂用量/µL	催化剂用量/µL	反应温度/℃	反应时间/h	6种苯氧羧酸类除草剂回收率之和
1	100	10	室温	2	2.151
2	100	20	40	3	4.495
3	100	30	60	4	4.134
4	200	10	40	4	4.476
5	200	20	60	2	3.610
6	200	30	室温	3	2.877
7	300	10	60	3	4.879
8	300	20	室温	4	3.390
9	300	30	40	2	5.426
均值1	3.593	3.835	2.806	3.729
均值2	3.654	3.832	4.799	4.084
均值3	4.565	4.146	4.208	4.000
极差	0.972	0.314	1.993	0.355

序号	化合物名称	曲线方程	相关系数
1	MCPA	y=1.84x＋0.010	0.9998
2	2,4-DP	y=2.54x＋0.041	0.9997
3	2,4-D	y=3.00x＋0.0084	0.9998
4	2,4,5-TP	y=2.72x＋0.036	0.9998
5	2,4,5-T	y=3.40x＋0.0065	0.9998
6	2,4-DB	y=8.30x＋0.039	0.9998