两种剂型吡唑醚菌酯在草莓中的残留及消解动态

doi:10.3969/j.issn.1004-1524.20220807

浙江农业学报 ›› 2023, Vol. 35 ›› Issue (7): 1720-1728.DOI: 10.3969/j.issn.1004-1524.20220807

两种剂型吡唑醚菌酯在草莓中的残留及消解动态

叶会¹^,²(), 陈瑜婷¹, 骆玉琴², 范续艳², 雷圆², 陆兰菲², 郝培培³, 程有普¹^,^*(), 张昌朋²^,^*()

1.天津农学院园艺园林学院,天津 300392
2.农业农村部农药残留检测重点实验室,浙江省农业科学院农产品质量安全与营养研究所,浙江杭州 310021
3.天津市绿亨化工有限公司,天津 300450

收稿日期:2022-05-31 出版日期:2023-07-25 发布日期:2023-08-17
作者简介:叶会(1996—),女,贵州安顺人,硕士研究生,研究方向为农药残留与农产品安全。E-mail: 827004242@qq.com
通讯作者: *程有普,E-mail: chengyoupu@tjau.edu.cn;
张昌朋,E-mail: cpzhang1215@zaas.ac.cn
基金资助:
浙江省基础公益研究计划(LGN21C140006);国家重点研发计划(2019YFC1605600)

Residue and dissipation dynamics of two formulations of pyraclostrobin in strawberry

YE Hui¹^,²(), CHEN Yuting¹, LUO Yuqin², FAN Xuyan², LEI Yuan², LU Lanfei², HAO Peipei³, CHENG Youpu¹^,^*(), ZHANG Changpeng²^,^*()

1. College of Horticulture and Landscape Architecture, Tianjin Agricultural University, Tianjin 300392, China
2. Key Laboratory for Pesticide Residue Detection, Ministry of Agriculture and Rural Affairs, Institute of Quality, Safety and Nutrition for Agro-Products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China
3. Tianjin Luheng Chemical Co., Ltd., Tianjin 300450, China

Received:2022-05-31 Online:2023-07-25 Published:2023-08-17
Contact: CHENG Youpu,ZHANG Changpeng

摘要/Abstract

摘要：

为明确吡唑醚菌酯乳油(EC)和微囊悬浮剂(CS)在草莓上的残留规律,分别以两种剂量(90 和150 g·hm^-2)于草莓成熟期施药,开展吡唑醚菌酯在草莓及土壤中的残留动态试验。结果表明,吡唑醚菌酯经QuEChERS-UPLC-MS/MS后的最低检测浓度分别为0.002 0(草莓和土壤)和0.005 0 mg·kg^-1(叶、茎和根)。在0.002~2 mg·kg^-1添加水平下,吡唑醚菌酯(草莓和土壤)的平均回收率为88%~110%,相对标准偏差(RSD)为1%~9%;在0.005~2 mg·kg^-1范围内,平均回收率(根、茎及叶)为74%~108%,RSD为2%~9%。残留试验结果表明,吡唑醚菌酯EC和CS施药1 d后在草莓中的残留分别为0.20~0.28 mg·kg^-1(90~150 g·hm^-2)和0.14~0.20 mg·kg^-1(90~150 g·hm^-2),残留量低于0.5 mg·kg^-1,均符合我国和欧盟在草莓中的限量值。吡唑醚菌酯仅在草莓、茎和叶的降解动态符合一级动力学模型,在草莓中的半衰期为6.6~6.8 d(EC)和7.7~9.8 d(CS),属于易降解农药。试验结果为微囊悬浮剂剂型吡唑醚菌酯在草莓体系上的安全使用提供了数据支持。

关键词: 吡唑醚菌酯, 微囊悬浮剂, 乳油, 农药残留

Abstract:

To clarify the residue patterns of pyraclostrobin on strawberry in the form of emulsifiable concentrate (EC) and microencapsulated suspension (CS), dynamic trials of pyraclostrobin residues in strawberry and soil were conducted at two doses (90 and 150 g·hm^-2) during ripening, respectively. The results showed that the minimal concentration of detection of pyraclostrobin based on QuEChERS-UPLC-MS/MS were 0.002 (strawberry and soil) and 0.005 mg·kg^-1 (leaf, stem and root), respectively. The average recoveries of pyraclostrobin (strawberry and soil) were 88%-110% with the relative standard deviations (RSDs) of 1%-9% at the spiked levels of 0.002-2 mg·kg^-1. The average recoveries (root, stem and leaf) in the range of 0.005-2 mg·kg^-1 were 74%-108% with RSDs of 2%-9%. The results of residue trials showed that the residues of pyraclostrobin in EC and CS in strawberry after 1 d of application were 0.20-0.28 mg·kg^-1 (90-150 g·hm^-2) and 0.14-0.20 mg·kg^-1 (90-150 g·hm^-2), respectively. The residues were lower than 0.5 mg·kg^-1, which were in accordance with the limit values of China and EU in strawberry. The degradation dynamics of pyraclostrobin only in strawberry, stem and leaf were in accordance with the first order kinetic model, and the half-lives in strawberry were 6.6-6.8 d (EC) and 7.7-9.8 d (CS), which were easily degradable pesticides. The trial results provided data to support the safe consumption of microencapsulated suspension dosage form of pyraclostrobin on strawberry.

Key words: pyraclostrobin, microcapsule suspension, emulsifiable concentrate, pesticide residue

中图分类号:

S481.8

叶会, 陈瑜婷, 骆玉琴, 范续艳, 雷圆, 陆兰菲, 郝培培, 程有普, 张昌朋. 两种剂型吡唑醚菌酯在草莓中的残留及消解动态[J]. 浙江农业学报, 2023, 35(7): 1720-1728.

YE Hui, CHEN Yuting, LUO Yuqin, FAN Xuyan, LEI Yuan, LU Lanfei, HAO Peipei, CHENG Youpu, ZHANG Changpeng. Residue and dissipation dynamics of two formulations of pyraclostrobin in strawberry[J]. Acta Agriculturae Zhejiangensis, 2023, 35(7): 1720-1728.

图/表 7

参考文献 26

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保留时间 Retention time/min	母离子 Precursor ion(m/z)	子离子 Product ion(m/z)	滞留时间 Dwell time/s	锥孔电压 Cone voltage/V	碰撞能 Collision energy/eV
1.51	388.01	197.03^*	0.061	18	28
	388.01	163.05	0.061	18	12

保留时间 Retention time/min	母离子 Precursor ion(m/z)	子离子 Product ion(m/z)	滞留时间 Dwell time/s	锥孔电压 Cone voltage/V	碰撞能 Collision energy/eV
1.51	388.01	197.03^*	0.061	18	28
	388.01	163.05	0.061	18	12

线性范围 Linear range/ (mg·L^-1)	基质 Matrix	回归方程 Regression equation	决定系数 Coefficient of determination	基质效应 ME	检出限 LOD/ (mg·L^-1)	定量限 LOQ/ (mg·kg^-1)
0.0005~0.1	乙腈Acetonitrile	y=1 938 010.57x+4 352.84	0.999 7	—	—	—
	叶Leaf	y=2 804 465.99x+1 0761.20	0.998 9	0.87	0.000 5	0.005 0
	茎Stem	y=2 576 648.62x+3 515.89	1.000 0	0.85	0.000 5	0.005 0
	草莓Strawberry	y=1 992 976.51x+6 239.22	0.999 2	1.03	0.000 5	0.002 0
	根Root	y=2 081 043.87x+6 103.10	0.999 8	1.07	0.000 5	0.005 0
	土壤Soil	y=2 292 365.17x+7 089.11	0.999 8	1.21	0.000 5	0.002 0

线性范围 Linear range/ (mg·L^-1)	基质 Matrix	回归方程 Regression equation	决定系数 Coefficient of determination	基质效应 ME	检出限 LOD/ (mg·L^-1)	定量限 LOQ/ (mg·kg^-1)
0.0005~0.1	乙腈Acetonitrile	y=1 938 010.57x+4 352.84	0.999 7	—	—	—
	叶Leaf	y=2 804 465.99x+1 0761.20	0.998 9	0.87	0.000 5	0.005 0
	茎Stem	y=2 576 648.62x+3 515.89	1.000 0	0.85	0.000 5	0.005 0
	草莓Strawberry	y=1 992 976.51x+6 239.22	0.999 2	1.03	0.000 5	0.002 0
	根Root	y=2 081 043.87x+6 103.10	0.999 8	1.07	0.000 5	0.005 0
	土壤Soil	y=2 292 365.17x+7 089.11	0.999 8	1.21	0.000 5	0.002 0

基质 Matrix	加标水平 Spike level/ (mg·kg^-1)	日内精密度Intra-day (n=5)/%						日间精密度Inter-day (n=15)/%
		1 d		2 d		3 d
		Rec	RSD	Rec	RSD	Rec	RSD	Rec		RSD
叶Leaf	0.005	89	8	89	4	87	5		89	8
	0.01	78	4	79	3	74	3		76	3
	2	83	5	80	6	79	5		81	3
茎Stem	0.005	91	9	97	8	92	9		93	9
	0.01	91	5	81	7	87	7		97	8
	2	77	4	83	5	86	5		91	9
草莓	0.002	96	3	97	1	96	4		97	4
Strawberry	0.01	94	3	96	4	88	2		107	3
	2	97	1	91	2	94	1		96	1
根Root	0.005	106	2	108	6	101	4		107	4
	0.01	96	6	94	6	101	5		105	5
	2	93	2	92	3	92	3		94	2
土壤Soil	0.002	110	9	105	6	101	6		104	7
	0.01	99	7	103	6	104	7		102	6
	2	99	4	95	3	97	4		94	4

两种剂型吡唑醚菌酯在草莓中的残留及消解动态

Residue and dissipation dynamics of two formulations of pyraclostrobin in strawberry

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剂型 Formulation	剂量 Dose/ (g·hm^-2)	时间 Time	草莓 Strawberry/ (mg·kg^-1)	叶 Leaf/ (mg·kg^-1)	茎 Stem/ (mg·kg^-1)	根 Root/ (mg·kg^-1)	土壤 Soil/ (mg·kg^-1)
乳油EC	90	2 h	0.25±0.01	7.83±0.12	1.64±0.04	0.11±0.01	0.02±0
		1 d	0.20±0.01	6.52±0.05	1.33±0.04	0.17±0.01	0.01±0
		3 d	0.14±0.01	5.53±0.01	1.27±0.02	0.07±0	0.01±0
		5 d	0.11±0	5.12±0.01	0.95±0.04	0.06±0	0.01±0
		7 d	0.10±0.01	4.69±0.30	0.87±0.66	0.04±0	0.01±0
		10 d	0.08±0.01	4.33±0.08	0.72±0.08	0.05±0	0.02±0
	150	2 h	0.27±0.01	9.75±0.05	2.12±0.07	0.22±0.01	0.02±0
		1 d	0.28±0.01	8.80±0.10	2.28±0.08	0.16±0	0.01±0
		3 d	0.25±0.01	8.12±0.14	1.83±0.07	0.11±0	0.02±0
		5 d	0.19±0.01	8.03±0.16	1.56±0.09	0.10±0.01	0.02±0
		7 d	0.14±0	7.30±0.29	1.12±0.06	0.08±0	0.02±0
		10 d	0.11±0	6.42±0.19	1.07±0.09	0.05±0	0.02±0
微囊悬浮剂CS	90	2 h	0.16±0	5.94±0.10	1.09±0.03	0.07±0	0.02±0
		1 d	0.14±0.01	5.10±0.01	0.92±0.09	0.07±0	0.02±0
		3 d	0.10±0.01	4.97±0.06	0.76±0.03	0.09±0	0.01±0
		5 d	0.10±0.01	4.62±0.16	0.69±0.06	0.05±0	0.02±0
		7 d	0.09±0.01	4.56±0.01	0.65±0.05	0.07±0.01	0.01±0
		10 d	0.06±0.01	3.57±0.01	0.60±0.03	0.03±0	0.02±0
	150	2 h	0.21±0.01	8.90±0.17	1.68±0.03	0.10±0.01	0.02±0
		1 d	0.20±0.01	8.53±0.14	1.62±0.06	0.14±0	0.03±0
		3 d	0.16±0.01	7.37±0.30	1.22±0.05	0.13±0.01	0.01±0
		5 d	0.16±0.01	7.25±0.22	1.16±0.01	0.07±0.01	0.02±0
		7 d	0.12±0.01	7.16±0.35	1.17±0.01	0.05±0.01	0.03±0
		10 d	0.10±0.01	6.48±0.35	0.94±0.06	0.04±0	0.03±0

剂型 Formulation	样品 Sample	回归方程 Regression equation		决定系数 Determination coefficient(R²)		半衰期 Half-life/d
剂型 Formulation	样品 Sample	90 g·hm^-2	150 g·hm^-2	90 g·hm^-2	150 g ·hm^-2	90 g ·hm^-2	150 g ·hm^-2
乳油EC	草莓Strawberry	C_t=0.212 6e^-0.1051^t	C_t=0.301 8e^-0.1015^t	0.923 5	0.925 6	6.6	6.8
	茎Stem	C_t=1.581 2e^-0.0814^t	C_t=2.268 7e^-0.0813^t	0.965 5	0.926 4	8.5	8.6
	叶Leaf	C_t=7.05 0e^-0.0550^t	C_t=9.419 3e^-0.0380^t	0.890 3	0.951 1	12.6	18.2
微囊悬浮剂	草莓Strawberry	C_t=0.148 7e^-0.0895^t	C_t=0.208 3e^-0.0708^t	0.929 3	0.947 4	7.7	9.8
CS	茎Stem	C_t=0.978 1e^-0.0558^t	C_t=1.615 6e^-0.0540^t	0.877 5	0.895 7	12.4	12.5
	叶Leaf	C_t=5.690 2e^-0.0423^t	C_t=8.612 2e^-0.0297^t	0.894 3	0.896 2	16.5	23.1

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