基于QuEChERS-GC/MS法对土壤和甜菜中精异丙甲草胺的残留降解动态测定

doi:10.6048/j.issn.1001-4330.2023.03.022

新疆农业科学 ›› 2023, Vol. 60 ›› Issue (3): 706-714.DOI: 10.6048/j.issn.1001-4330.2023.03.022

• 植物保护·设施农业·农产品加工工程·微生物 • 上一篇下一篇

基于QuEChERS-GC/MS法对土壤和甜菜中精异丙甲草胺的残留降解动态测定

程文亮(), 宋文钰, 王浩东, 许同心, 吴彩兰, 王春娟(), 杨德松()

石河子大学农学院/新疆绿洲农业病虫害治理与植保资源利用重点实验室,新疆石河子 832000

收稿日期:2022-09-03 出版日期:2023-03-20 发布日期:2023-04-18
通信作者: 王春娟(1979-),女,讲师,博士,研究方向为生物农药,(E-mail)wchunjuan@126.com;
杨德松(1977-),男,安徽滁州人,教授,博士,硕士生导师,研究方向为农药环境毒理学,(E-mail)yds_agr@shzu.edu.cn
作者简介:程文亮(1997-),男,河南周口人,硕士研究生,研究方向为农药毒理学,(E-mail)1426088390@qq.com
基金资助:
新疆生产建设兵团重大科技计划“机采棉田杂草高效防除技术研发与集成应用”(2018AA006)

Determination of Residual Degradation of S-Metolachor Residue in Soil and Sugar Beet by QuEChERS-GC/MS

CHENG Wenliang(), SONG Wenyu, WANG Haodong, XU Tongxin, WU Cailan, WANG Chunjuan(), YANG Desong()

Key Laboratory for Oasis Agricultural Pest Management and Plant Protection Resource Utilization / College of Agronomy, Shihezi University, Shihezi Xinjiang 832003,China

Received:2022-09-03 Online:2023-03-20 Published:2023-04-18
Correspondence author: WANG Chunjuan(1979-), Female, Ph.D., lecturer, Research field: biological pesticide research,(E-mail)wchunjuan@126.com;
YANG Desong(1977-), Male, Ph.D., Professor, Master instutor, Research field: pesticide toxicology research, (E-mail)yds_agr@shzu.edu.cn
Supported by:
Major Scientific R & D Program Project of XPCC "Research and Development and Integrated Application of Efficient Weed Control Technology in Machine-picked Cotton Field"(2018AA006)

摘要/Abstract

摘要：

【目的】研究精异丙甲草胺在甜菜及种植土壤中的残留降解动态。【方法】采用QuEChERS-GC/MS法,分析不同深度土壤和甜菜中施用的不同浓度的精异丙甲草胺。【结果】精异丙甲草胺在0.01~1.0 mg/L浓度范围内呈良好线性,相关系数为0.999 4,所建立的最小检出限为0.001 mg/kg;平均回收率在84.81%~110.45%,相对标准偏差(RSD,n=3)在1.36%~9.0%。1 296、1 944、3 888 g.a.i/hm²的精异丙甲草胺在0~5、5~10、10~15 cm的土壤以及甜菜中的降解遵循一级动力学方程,不同深度土壤中的残留量随浓度的增加而增加,随时间的延长而降低,不同施用浓度在不同深度土壤中的半衰期为9.12~17.77 d。施用浓度越高,降解速度越慢。在甜菜中的残留量和降解速率都低于土壤,半衰期较土壤中略高,3个浓度在甜菜中的半衰期分别为19.25、26.65和32.85 d。【结论】施用1 296和1 944 g.a.i/hm²的精异丙甲草胺,收获期在土壤和甜菜中的降解率均能达到90%;施用超剂量3 888 g.a.i/hm²的精异丙甲草胺在收获期的降解率会低于80%,精异丙甲草胺在土壤和甜菜中较易降解,属于易降解农药。

关键词: 精异丙甲草胺; 土壤; 甜菜; QuEChERS-GC/MS; 降解动态

Abstract:

【Objective】 This project aims to clarify the residual degradation dynamics of metolachlor in sugar beet and planting soil.【Method】 QuEChERS-GC/MS method was used to study the effects of different concentrations of S-Metolachor in different soil depths and sugarbeet.【Results】 The results showed that the S-Metolachorresidue was linear in the concentration range of 0.01-1.0 mg/L with a correlation coefficient of 0.999 4.The minimum detection limit was 0.001 mg/kg; the average recovery was 84.81-110.45%, relative standard deviation (RSD, n=3) was between 1.36% and 9.0%.The degradation of S-Metolachorresidue in 0-5, 5-10, 10-15 cm soil and sugar beet in 1,296, 1,944, 3,888 g.a.i/hm², following the first-order kinetic equation.The residue in different depth soil increased with the increase of concentration, and decreased with the extension of time.The half-life of different application concentration in different depth soil was 9.12-17.77 d.The higher the application concentration, the slower the degradation rate.The residual amount and degradation rate in sugar beet were lower than that in soil, and the half-life was slightly higher than that in soil.The half-lives of three concentrations in sugar beet were 19.25 d, 26.65 d and 32.85 d, respectively.【Conclusion】 The degradation rate of S-Metolachlor in soil and sugar beet can reach 90% when 1,296 g.a.i/hm² and 1,944 g.a.i/hm² are applied, and is lower than 80% when the dosage of S-Metolachlor is 3,888 g.a.i/hm².From the perspective of degradation rate, S-Metolachlor is easy to degrade in soil and sugar beet, which belongs a kind of degradable pesticide.

Key words: S-Metolachor; soil; sugar beet; QuEChERS-GC/MS; degradation dynamics

中图分类号:

S566.3

程文亮, 宋文钰, 王浩东, 许同心, 吴彩兰, 王春娟, 杨德松. 基于QuEChERS-GC/MS法对土壤和甜菜中精异丙甲草胺的残留降解动态测定[J]. 新疆农业科学, 2023, 60(3): 706-714.

CHENG Wenliang, SONG Wenyu, WANG Haodong, XU Tongxin, WU Cailan, WANG Chunjuan, YANG Desong. Determination of Residual Degradation of S-Metolachor Residue in Soil and Sugar Beet by QuEChERS-GC/MS[J]. Xinjiang Agricultural Sciences, 2023, 60(3): 706-714.

图/表 9

参考文献 20

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样品 Sam- ple	添加水平 Addition level (μg/mL)	回收率 Recovery (%)			平均回收率 Average recovery (%)	相对标准偏差 Relative standard deviation (%)
土壤 Soil	0.10	77.93	87.95	88.56	84.81	7.04
	0.50	82.20	88.03	90.62	86.95	4.96
	1.00	92.42	95.38	98.42	95.41	3.14
甜菜 Sugar beet	0.10	99.48	101.52	98.95	99.98	1.36
	0.50	120.51	110.21	100.64	110.45	9.00
	1.00	102.50	99.84	100.03	100.79	1.47

样品 Sam- ple	添加水平 Addition level (μg/mL)	回收率 Recovery (%)			平均回收率 Average recovery (%)	相对标准偏差 Relative standard deviation (%)
土壤 Soil	0.10	77.93	87.95	88.56	84.81	7.04
	0.50	82.20	88.03	90.62	86.95	4.96
	1.00	92.42	95.38	98.42	95.41	3.14
甜菜 Sugar beet	0.10	99.48	101.52	98.95	99.98	1.36
	0.50	120.51	110.21	100.64	110.45	9.00
	1.00	102.50	99.84	100.03	100.79	1.47

深度 Depth (cm)	浓度 Concentration (g.a.i/hm²)	消解方程 Digestion equation	K	R²	半衰期 Half-life (d)
0~5	1 296	Y=3.869 e^-0^.⁰⁶⁵^t	0.065	0.891 3	10.66
	1 988	Y=4.821 e^-0^.⁰⁵⁹^t	0.059	0.900 5	11.75
	3 888	Y=7.283 e^-0^.⁰⁶⁴^t	0.064	0.970 5	10.83
5~10	1 296	Y=0.797 e^-0^.⁰⁵⁷^t	0.057	0.965 9	12.16
	1 988	Y=1.661 e^-0^.⁰⁴³^t	0.043	0.966 4	16.12
	3 888	Y=6.254 e^-0^.⁰⁷⁶^t	0.076	0.956 1	9.12
10~15	1 296	Y=0.491 e^-0^.⁰⁶¹^t	0.061	0.978 7	11.36
	1 988	Y=0.991 e^-0^.⁰³⁹^t	0.039	0.943 0	17.77
	3 888	Y=0.706 e^-0^.⁰⁵³^t	0.053	0.985 3	13.08

深度 Depth (cm)	浓度 Concentration (g.a.i/hm²)	消解方程 Digestion equation	K	R²	半衰期 Half-life (d)
0~5	1 296	Y=3.869 e^-0^.⁰⁶⁵^t	0.065	0.891 3	10.66
	1 988	Y=4.821 e^-0^.⁰⁵⁹^t	0.059	0.900 5	11.75
	3 888	Y=7.283 e^-0^.⁰⁶⁴^t	0.064	0.970 5	10.83
5~10	1 296	Y=0.797 e^-0^.⁰⁵⁷^t	0.057	0.965 9	12.16
	1 988	Y=1.661 e^-0^.⁰⁴³^t	0.043	0.966 4	16.12
	3 888	Y=6.254 e^-0^.⁰⁷⁶^t	0.076	0.956 1	9.12
10~15	1 296	Y=0.491 e^-0^.⁰⁶¹^t	0.061	0.978 7	11.36
	1 988	Y=0.991 e^-0^.⁰³⁹^t	0.039	0.943 0	17.77
	3 888	Y=0.706 e^-0^.⁰⁵³^t	0.053	0.985 3	13.08

时间 Time	消解率 Digestion rate	深度 Depth 0~5 (cm)			深度 Depth 5~10 (cm)			深度 Depth 10~15 (cm)
		浓度 Concentration (g.a.i/hm²)
		1 296	1 944	3 888	1 296	1 944	3 888	1 296	1 944	3 888
施药后1 d 1 d after application	w/(mg/kg)	5.00	6.40	8.75	0.56	0.75	6.56	0.26	0.31	0.32
施药后7 d 7 d after application	w/(mg/kg)	3.31	4.15	5.01	0.79	0.98	7.74	0.41	0.36	0.42
施药后7 d 7 d after application	消解率(%)	33.60	35.11	42.79	-	-	-	-	-	-
施药后14 d 14 d after application	w/(mg/kg)	2.15	2.89	3.24	0.54	0.75	3.86	0.26	0.53	0.72
施药后14 d 14 d after application	消解率(%)	56.94	54.87	63.03	4.10	0.53	41.10	-	-	-
施药后21 d 21 d after application	w/(mg/kg)	1.07	1.34	2.06	0.27	0.74	2.55	0.25	0.41	0.50
施药后21 d 21 d after application	消解率(%)	78.68	79.01	76.43	51.52	1.33	61.19	2.70	-	-
施药后30 d 30 d after application	w/(mg/kg)	0.44	0.67	1.04	0.25	0.47	1.04	0.17	0.24	0.28
施药后30 d 30 d after application	消解率(%)	91.31	89.46	88.07	55.79	37.33	84.19	32.82	20.92	14.81
施药后45 d 45 d after application	w/(mg/kg)	0.09	0.12	0.23	0.16	0.29	0.33	0.09	0.23	0.25
施药后45 d 45 d after application	消解率(%)	98.22	98.15	97.40	71.84	61.33	95.00	66.02	23.53	22.84
施药后60 d 60 d after application	w/(mg/kg)	0.03	0.08	0.19	0.09	0.212	0.20	0.03	0.13	0.15
施药后60 d 60 d after application	消解率(%)	99.41	98.74	98.65	83.96	71.73	96.94	90.35	56.21	53.09
施药后90 d 90 d after application	w/(mg/kg)	0.03	0.06	0.11	0.02	0.02	0.09	0.01	0.02	0.07
施药后90 d 90 d after application	消解率(%)	99.33	99.13	98.76	96.43	97.07	98.60	94.98	92.81	79.63

基于QuEChERS-GC/MS法对土壤和甜菜中精异丙甲草胺的残留降解动态测定

Determination of Residual Degradation of S-Metolachor Residue in Soil and Sugar Beet by QuEChERS-GC/MS

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Metrics

浓度 Concen tration (g.a.i/hm²)	消解方程 Digestion equation	K	R²	半衰期 Half-life (d)
1 296	Y=0.045 9e^-0^.⁰³⁶^t	0.036	0.950 3	19.25
1 988	Y=0.050 7e^-0^.⁰²⁶^t	0.026	0.991 7	26.65
3 888	Y=0.063 4e^-0^.⁰²¹^t	0.021	0.946 4	32.85

时间 Time	消解率 Digestion rate(%)	浓度 Concentration (g.a.i/hm²)
时间 Time	消解率 Digestion rate(%)	1 296	1 944	3 888
第一次采样0 d First sampling 0 d	w(mg/kg)	0.036	0.042	0.052
间隔10 d Interval 10 d	w(mg/kg)	0.029	0.039	0.050
间隔10 d Interval 10 d	消解率(%)	21.700	13.690	5.160
间隔20 d Interval 20 d	w(mg/kg)	0.024	0.034	0.049
间隔20 d Interval 20 d	消解率(%)	35.440	24.720	7.270
间隔30 d Interval 30 d	w(mg/kg)	0.019	0.023	0.036
间隔30 d Interval 30 d	消解率(%)	48.080	48.790	31.930
间隔40 d Interval 40 d	w(mg/kg)	0.012	0.019	0.028
间隔40 d Interval 40 d	消解率(%)	66.480	57.620	46.080
间隔60 d Interval 60 d	w(mg/kg)	0.008	0.011	0.022
间隔60 d Interval 60 d	消解率(%)	78.300	76.600	57.170
收获期采样 Harvest sampling	w(mg/kg)	0.001	0.005	0.008
收获期采样 Harvest sampling	消解率(%)	96.430	89.400	84.510

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