Determination of 2 Strobilurin Fungicide Residues in Soil by Modified QuEChERS Method Combined with Liquid Chromatography

doi:10.11924/j.issn.1000-6850.casb2023-0467

Abstract

Abstract:

The study aimed at establishing a high performance liquid chromatography (HPLC) method for the determination of pyraclostrobin and kresoxim-methyl in three different types of soil from Xinjiang, Inner Mongolia and Heilongjiang. The separation of pyraclostrobin or kresoxim-methyl in samples was performed by modified QuEChERS method combined with HPLC, and the quantitative results were calculated by external standard method. The results showed good linearity in the concentration ranged from 0.3-10.0 mg/L, and the correlation coefficient (R²) was greater than 0.9999. At different concentrations, the average recoveries of pyraclostrobin and kresoxim-methyl in Yermosols of Xinjiang were 98.03%-102.32% and 100.33%-107.18% with relative standard deviations (RSD) of 0.46%-0.87% and 0.94%-1.67%. The average recoveries of pyraclostrobin and kresoxim-methyl in Chernozem of Heilongjiang were 100.40%-104.32% and 90.83%-101.33% with RSD of 0.47%-2.78% and 1.35%-1.69%. The average recoveries of pyraclostrobin and kresoxim-methyl in Xerosols of Inner Mongolia were 100.04%-107.40% and 96.90%-98.86% with RSD of 0.77%-1.41% and 1.08%-1.57%. The accuracy and precision of the method meet the requirements of pesticide residue analysis, and it is suitable for the determination of pyraclostrobin and kresoxim-methyl in above types of soil.

Key words: pyraclostrobin, kresoximm-methyl, high performance liquid chromatography (HPLC), soil, residue analysis

DING Yuling, TONG Menglu, PANG Caiwei, JIANG Bingshan, WANG Zichen, ZHOU Qin. Determination of 2 Strobilurin Fungicide Residues in Soil by Modified QuEChERS Method Combined with Liquid Chromatography[J]. Chinese Agricultural Science Bulletin, 2024, 40(5): 127-134.

Figures/Tables 8

References 40

[1]	喻歆茹, 路彩红, 徐玲英, 等. GC-MS/MS法测定草莓中吡唑醚菌酯残留量及安全评价[J]. 植物保护, 2021, 47(4):141-147.
[2]	张凯, 范龙涛, 彭效明, 等. 吡唑醚菌酯合成研究进展[J]. 现代农药, 2018, 17(2):8-11.
[3]	罗跃, 吴小毛, 胡贤锋, 等. 吡唑醚菌酯的降解代谢及毒理研究进展[J]. 农业资源与环境学报, 2022, 39(4):651-663.
[4]	蔡光辉, 李萌, 吴绪金, 等. 吡唑醚菌酯在杨桃中残留检测及膳食风险评估[J]. 食品安全质量检测学报, 2021, 12(14):5531-5539.
[5]	LI P P, SUN P Y, LI D, et al. Evaluation of pyraclostrobin as an ingredient for soybean seed treatment by analyzing its accumulation-dissipation kinetics, plant-growth activation, and protection against Phytophthora sojae[J]. Journal of agricultural and food chemistry, 2020, 68(43):11928-11938. doi: 10.1021/acs.jafc.0c04376 URL
[6]	骆琴, 周宇杰, 何信富. 芸苔素内酯与吡唑醚菌酯对水稻抗病性及产量的影响[J]. 中国稻米, 2020, 26(1):72-74. doi: 10.3969/j.issn.1006-8082.2020.01.016
[7]	任学祥, 苏贤岩, 范富云, 等. 吡唑醚菌酯在小麦不同生育期病害防治中的应用[J]. 农药学学报, 2023(1):89-96.
[8]	郭宁, 于淑晶, 孙华, 等. 不同配方吡唑醚菌酯包衣对玉米茎腐病的防治试验[J]. 农药, 2023(2):154-156.
[9]	SHARMA P, MALVICK D K, CHANDA A K, et al. Sensitivity of Rhizoctonia solani anastomosis group 2-2 isolates from soybean and sugar beet to selected SDHI and QoI fungicides[J]. Plant disease, 2021, 105(11):3573-3579. doi: 10.1094/PDIS-12-20-2680-RE URL
[10]	MALHAT F, ANAGNOSTOPOULOS C, SABER E, et al. Dissipation kinetics and risk assessment of pyraclostrobin after open field application in cucumber under Egyptian conditions[J]. Journal of consumer protection and food safety, 2021, 16(4):333-341. doi: 10.1007/s00003-021-01330-4
[11]	MESARA S N, DAVE K P, SUBRAMANIAN R B. Comparative transcriptome analysis elucidates positive physiological effects of foliar application of pyraclostrobin on tomato (Solanum lycopersicum L.)[J]. Physiology and molecular biology of plants, 2022(5):971-986.
[12]	ODILBEKOV F, EDIN E, MOSTAFANEZHAD H, et al. Within-season changes in Alternaria solani populations in potato in response to fungicide application strategies[J]. European journal of plant pathology, 2019, 155(3): 953-965. doi: 10.1007/s10658-019-01826-8
[13]	刘霞, 罗灵芝, 吴燕, 等. 吡唑醚菌酯和克菌丹在苹果上的残留特性及风险评估[J]. 生态毒理学报, 2021(6):327-334.
[14]	YU X R, LU C H, XU L Y, et al. Residue analysis and safety evaluation of pyraclostrobin in strawberry by GC-MS/MS[J]. Plant protection, 2021, 47(4):141-147.
[15]	李建明, 何莲, 孔玄庆, 等. 苯醚甲环唑和吡唑醚菌酯对柑橘炭疽病菌的联合毒力及防效[J]. 现代农药, 2022, 21(5):60-64.
[16]	孙东晗, 陈悦, 田文学, 等. 吉林省西瓜蔓枯病菌对吡唑醚菌酯的抗性监测及抗性风险评估[J]. 植物保护学报, 2022(6):1663-1672.
[17]	李婷, 董雪娟, 赵霞, 等. 吡唑醚菌酯、乙嘧酚磺酸酯和乙嘧酚在葡萄中的残留消解及膳食风险评估[J]. 农产品质量与安全, 2022(6):63-67.
[18]	张景朋, 张卿硕, 蒋明亮, 等. 醚菌酯高效液相色谱分析方法及其防腐材抗流失性能研究[J]. 木材科学与技术, 2023, 37(2):66-71.
[19]	李彩霞, 蔡云梅. 醚菌酯在黄瓜和土壤中的残留及消解动态研究[J]. 安徽农业科学, 2020, 48(22):87-89,98.
[20]	孔肖, 闫晓静, 杨代斌, 等. 丙环唑和醚菌酯药液浓度、雾滴密度与其对小麦白粉病防效的关系[J]. 农药学学报, 2018(3):301-308.
[21]	DONG C, HU J Y. Residue levels and dietary risk evaluation of prothioconazole-desthio and kresoxim-methyl in cucumbers after field application in twelve regions in China[J]. Food additives and contaminants part a-chemistry analysis control exposure & risk assessment, 2023, 40(4):566-575.
[22]	刘梦竹, 裴鸿艳, 张静, 等. 大豆锈病防治药剂研究进展[J]. 现代农药, 2020, 19(6):11-21.
[23]	翟赛亚, 李红艳. 防治小麦锈病的药效试验研究[J]. 河南农业, 2020(20):22-23.
[24]	王莉莉, 徐建强, 朱凯, 等. 醚菌酯对假禾谷镰孢的抑制作用及对小麦茎基腐病的防效研究[J]. 植物病理学报, 2022(3):434-442.
[25]	赵琪君, 刘世江, 丁怡, 等. 稻瘟病菌对丙环唑和醚菌酯的敏感性检测[J]. 农药, 2019, 58(6):462-464,468.
[26]	LI B X, WANG W C, ZHANG X P, et al. Using coordination assembly as the microencapsulation strategy to promote the efficacy and environmental safety of pyraclostrobin[J]. Advanced functional materials, 2017, 27(29):1701841. doi: 10.1002/adfm.v27.29 URL
[27]	朱卫芳, 黄兰淇, 张颂函, 等. 25%吡唑醚菌酯悬浮剂在蓝莓中的残留行为及膳食风险评估[J]. 农药科学与管理, 2023, 44(1):47-53.
[28]	叶倩, 朱富伟, 万凯, 等. LC-MS/MS测定3种复合蔬果汁中吡唑醚菌酯、啶虫脒及哒螨灵残留[J]. 中国农学通报, 2022, 38(36):146-151. doi: 10.11924/j.issn.1000-6850.casb2022-0147
[29]	WANG S W, SUN H B, LIU Y P, et al. The disappearance behavior, residue distribution, and risk assessment of kresoxim-methyl in banana (Musa nana Lour.) based on a modified QuEChERS procedure using HPLC-MS/MS[J]. Frontiers in environmental science, 2022,10.
[30]	义国通, 陆燕, 农时锋. 气相色谱法同时测定火龙果中三唑酮·异菌脲和醚菌酯残留[J]. 安徽农业科学, 2020, 48(10):171-172,177.
[31]	李萌, 汪红, 马婧玮, 等. 水果中吡唑醚菌酯残留量检测及膳食摄入风险评估[J]. 中国果树, 2023(4):107-113.
[32]	CAO X, HE B C, LIU F, et al. Design, synthesis and bioactivity of myricetin derivatives for control of fungal disease and tobacco mosaic virus disease[J]. Sc advances, 2023, 13(10): 6459-6465.
[33]	宋晓兵, 黄峰, 罗小玲, 等. 吡唑醚菌酯对两种优稀水果病原菌的毒力测定及田间防治效果[J]. 中国农学通报, 2022, 38(27):125-128. doi: 10.11924/j.issn.1000-6850.casb2021-0996
[34]	POLAT Z, BAYRAKTAR H. Resistance of Venturia inaequalis to multiple fungicides in Turkish apple orchards[J]. Journal of phytopathology, 2021, 169(6): 360-368. doi: 10.1111/jph.v169.6 URL
[35]	姚锦爱, 赖宝春, 黄鹏, 等. 福建省草莓炭疽病菌对吡唑醚菌酯的敏感性及与其他药剂的交互抗性[J]. 植物保护学报, 2022(4):1263-1268.
[36]	胡传鹤, 李永涛, 尚梦如, 等. 5种新烟碱类农药在农田土壤中的吸附和淋溶行为[J]. 农业环境科学学报, 2023, 42(3):539-546.
[37]	ZHANG G, LIU Y, ZHENG S, et al. Efficient removal of formaldehyde by diatomite decorated with BiOCl/TiO₂ under visible-light irradiation: effects of key preparation parameters[J]. Advanced powder technology, 2021, 32(11):4364-4372. doi: 10.1016/j.apt.2021.09.041 URL
[38]	李栋, 李平亮, 李保华, 等. QuEChERS-高效液相色谱法分析6-苄氨基腺嘌呤和吡唑醚菌酯在番茄植株和土壤中的残留动态[J]. 农药学学报, 2020(1):97-104.
[39]	李金萍. 40%戊唑·醚菌酯悬浮剂的高效液相色谱分析[J]. 现代农药, 2015, 14(4):23-25.
[40]	李艳, 滕应, 赵玲, 等. QuEChERS-高效液相色谱法测定土壤中嘧霉胺和吡唑醚菌酯残留[J]. 农药, 2017(8):596-599.

土壤类型	pH	碱解氮/(mg/kg)	速效磷/(mg/kg)	速效钾/(mg/kg)	有机质/(g/kg)
新疆灰漠土	7.10	50.86	62.87	335.25	14.2
内蒙棕钙土	7.48	72.43	18.83	150.50	17.6
黑龙江黑钙土	6.45	189.88	37.22	336.25	52.8

土壤类型	pH	碱解氮/(mg/kg)	速效磷/(mg/kg)	速效钾/(mg/kg)	有机质/(g/kg)
新疆灰漠土	7.10	50.86	62.87	335.25	14.2
内蒙棕钙土	7.48	72.43	18.83	150.50	17.6
黑龙江黑钙土	6.45	189.88	37.22	336.25	52.8

土壤名称	吡唑醚菌酯			醚菌酯
土壤名称	添加浓度/ (mg/kg)	平均回收率/ %	相对标准偏差(RSD)/ %	添加浓度/ (mg/kg)	平均回收率/ %	相对标准偏差 (RSD)/%
新疆灰漠土	0.5	98.03	0.46	0.5	107.18	1.22
	1	102.32	0.86	1	103.17	0.94
	2	100.80	0.87	2	100.33	1.67
黑龙江黑钙土	0.5	104.32	2.78	0.5	90.83	1.35
	1	102.07	1.02	1	100.34	1.69
	2	100.04	0.47	2	101.33	1.49
内蒙棕钙土	0.5	107.40	1.25	0.5	97.03	1.08
	1	103.88	1.41	1	98.86	1.30
	2	100.04	0.77	2	96.90	1.57

土壤名称	吡唑醚菌酯			醚菌酯
土壤名称	添加浓度/ (mg/kg)	平均回收率/ %	相对标准偏差(RSD)/ %	添加浓度/ (mg/kg)	平均回收率/ %	相对标准偏差 (RSD)/%
新疆灰漠土	0.5	98.03	0.46	0.5	107.18	1.22
	1	102.32	0.86	1	103.17	0.94
	2	100.80	0.87	2	100.33	1.67
黑龙江黑钙土	0.5	104.32	2.78	0.5	90.83	1.35
	1	102.07	1.02	1	100.34	1.69
	2	100.04	0.47	2	101.33	1.49
内蒙棕钙土	0.5	107.40	1.25	0.5	97.03	1.08
	1	103.88	1.41	1	98.86	1.30
	2	100.04	0.77	2	96.90	1.57

土壤名称	添加浓度/(mg/kg)	标准溶液/%	BZM-A1/%	BZM-A2/%	BZM-A3/%	BZM-A4/%	BZM-A5/%	平均回收率/%
新疆灰漠土	0.5	98.20	98.00	98.00	97.70	97.50	98.80	98.03
	1	102.60	101.85	102.45	103.8	101.2	102	102.32
	2	100.85	100.05	101.8	101.45	101.18	99.48	100.80
黑龙江黑钙土	0.5	104.30	104.00	104.80	106.90	106.90	99.00	104.32
	1	102.15	100.05	102.05	102.60	102.90	102.70	102.07
	2	100.90	100.60	99.35	100.62	99.70	99.05	100.04
内蒙棕钙土	0.5	106.30	108.40	109.30	107.60	107.20	105.60	107.40
	1	102.05	102.85	103.35	104.10	104.75	106.20	103.88
	2	100.90	100.60	99.35	100.62	99.70	99.05	100.04