Residue Behavior of Thiamethoxam in Chinese Flowering Cabbage Analyzed by Performance Liquid Chromatography-tandem Mass Spectrometry

doi:10.11924/j.issn.1000-6850.casb2021-0552

Abstract

Abstract:

In order to research the residue behavior of thiamethoxam in Chinese flowering cabbage, the final residue trials of thiamethoxam in Chinese flowering cabbage were carried out in five provinces and one city, and the dissipation dynamic trials were carried out in two provinces. Samples were purified by solid phase extraction column, detected by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), and quantified by external standard method. The results showed that the recoveries of thiamethoxam and its metabolite clothianidin were 89%-102% and 93%-100%, and the relative standard deviations (RSDs) were 5.8%-8.5% and 4.0%-9.5%, under the spiked levels of 0.01-1 mg/kg. The limit of quantification (LOQ) of thiamethoxam and its metabolite clothianidin was 0.01 mg/kg. The half-lives of thiamethoxam in Chinese flowering cabbage were 1.2 and 1.8 days in Shandong Province and Anhui Province, respectively. The results of final residue trials in five provinces and one city showed that the residue level of thiamethoxam in Chinese flowering cabbage was <LOQ~0.125mg/kg 10 days after application when the dosage was 56.25-84.375 g a.i./hm² and the application was 2 to 3 times. The recommended application of 25% thiamethoxam WG to control Phyllotreta striolata in Chinese flowering cabbage was 2 times at the maximum dosage of 56.25 a.i.g/hm² with a safe interval of 7 days.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), thiamethoxam, Chinese flowering cabbage, residue, application safety assessment

LI Rumei, LIU Tongjin, LIANG Hui, FENG Yizhi, LIANG Lin, LI Ruijuan, YU Jianlei. Residue Behavior of Thiamethoxam in Chinese Flowering Cabbage Analyzed by Performance Liquid Chromatography-tandem Mass Spectrometry[J]. Chinese Agricultural Science Bulletin, 2023, 39(20): 133-137.

Figures/Tables 2

References 24

[1]	廖林慧, 王娣, 张昌朋, 等. 阿维菌素和噻虫嗪在豇豆不同生长时期施药后的降解代谢[J]. 浙江农业科学, 2020, 61(3):433-436.
[2]	宋超, 李海萍, 刘万峰, 等. 高效液相色谱法检测烟草中噻虫嗪残留及消解动态[J]. 农药学学报, 2014, 16(4):477-482.
[3]	刘同金, 李瑞娟, 宋国春, 等. 吡虫啉在花生田环境中的残留行为及安全评价[J]. 湖北农业科学, 2018, 57(16):57-61,65.
[4]	食品安全国家标准食品中农药最大残留限量:GB/T 2763—2019[S]. 北京: 中国标准出版社, 2019.
[5]	PANG N, FAN X, FANTKE P, et al. Dynamics and dietary risk assessment of thiamethoxam in wheat, lettuce and tomato using field experiments and computational simulation[J]. Environmental pollution, 2020, 256:113285. doi: 10.1016/j.envpol.2019.113285 URL
[6]	HE M, SONG D, JIA H C, et al. Concentration and dissipation of chlorantraniliprole and thiamethoxam residues in maize straw, maize, and soil[J]. Journal of environment science health (part B), 2016, 51(9):594-601.
[7]	李迎东, 侯新港, 齐颖慧, 等. QuEChERS结合高效液相色谱串联质谱法同时测定马铃薯中的噻虫嗪、氟啶虫酰胺及其代谢物[J]. 农药, 2019, 58(3):199-203.
[8]	刘炎, 欧阳迪庆, 叶玉凤, 等. QuEChERS结合超高效液相色谱-串联质谱法同时测定番茄中噻虫嗪、噻虫胺、螺虫乙酯及其代谢物残留[J]. 分析测试学报, 2017, 36(12):1431-1438.
[9]	梦云, 巩文雯, 刘庆菊, 等. 噻虫嗪及其代谢产物在盆栽辣椒和土壤中的残留动态和膳食风险评估[J]. 农药, 2018, 57(9):662-665.
[10]	戈文学, 杨宝东, 张志勇, 等. 噻虫嗪在苹果上的残留消解动态及膳食风险评估[J]. 农药, 2015, 54(2):115-118.
[11]	贺敏, 贾春虹, 王东, 等. 25%噻虫嗪水分散粒剂在青葱和大葱上的残留与安全性评价[J]. 食品安全质量检测学报, 2021, 12(2):609-615.
[12]	王博, 侯志广, 方楠, 等. 噻虫嗪及其代谢物在大葱中的消解动态及最终残留[J]. 农药, 2018, 57(9):671-674.
[13]	郇志博, 罗金辉, 谢德芳. 噻虫嗪在甘蔗和土壤中的残留行为及风险评估[J]. 南方农业学报, 2018, 49(11):2282-2291.
[14]	刘艳萍, 王思威, 孙海滨, 等. 噻虫嗪及其代谢物噻虫胺在节瓜中的消解动态及初步膳食风险评估[J]. 农药学学报, 2018, 20(2):211-216.
[15]	朱富伟, 叶倩, 黄玉芬, 等. 噻虫嗪及其代谢物噻虫胺在苦瓜上的残留及膳食风险评估[J]. 西北农林科技大学学报, 2020, 48(10):92-98.
[16]	刘同金, 李瑞娟, 冯义志, 等. 噻虫嗪在菜豆中的残留及安全性评价[J]. 浙江农业科学, 2020, 61(9):1854-1857.
[17]	冯义志, 潘金菊, 齐晓雪, 等. 噻虫嗪及其代谢产物噻虫胺在韭菜和土壤中的残留消解动态及残留量[J]. 现代农药, 2016, 15(5):45-48.
[18]	周力, 吴亚玉, 韩帅兵, 等. 噻虫嗪及其代谢产物噻虫胺在冬枣中的残留动态研究[J]. 农药科学与管理, 2019, 40(5):42-47.
[19]	陈仕军, 黄爱政, 温健新. 华南地区中晚熟菜心冬季品种比较试验[J]. 长江蔬菜, 2011(22):28-29.
[20]	陈兆贵, 王愈. 菜心ISSR分子标记技术初步研究[J]. 种子, 2010, 29(3):29-32.
[21]	钟玉娟, 张白鸽, 罗少波, 等. 菜薹硝酸盐积累与品种、营养品质之间的关系[J]. 中国农学通报, 2017, 33(18):49-55. doi: 10.11924/j.issn.1000-6850.casb16070140
[22]	张效宁, 孟祥哲, 逯晓楠, 等. 11个菜薹品种在山西晋中的引种栽培试验[J]. 山西农业科学, 2020, 49(1):46-49,53.
[23]	农作物中农药残留试验准则:NY/T 788—2018[S]. 北京: 中国标准出版社, 2018.
[24]	王运浩. 农药登记残留田间试验标准操作规程[M]. 北京: 中国标准出版社, 2007:275-279.

时间/d	山东省				安徽省
	残留量/(mg/kg)			消解率/%	残留量/(mg/kg)			消解率/%
	噻虫嗪	噻虫胺	噻虫嗪总和	消解率/%	噻虫嗪	噻虫胺	噻虫嗪总和	消解率/%
0.083	3.13	<0.01	3.14		2.04	0.0146	2.05
1	2.13	0.132	2.28	27.2	1.51	0.173	1.72	16.3
2	1.38	0.121	1.52	51.5	0.499	0.0464	0.553	73.0
3	0.951	0.0926	1.06	66.3	0.326	0.0213	0.351	82.9
5	0.440	0.0470	0.495	84.2	0.135	0.0136	0.151	92.6
7	0.195	0.0298	0.230	92.7	0.0324	<0.01	0.0424	97.9
14	<0.01	<0.01	<0.02		<0.01	<0.01	<0.02
21	<0.01	<0.01	<0.02		<0.01	<0.01	<0.02
方程	C=3.28e^-0.3789^T				C=2.2209e^-0.5651^T
R²	0.9999				0.9813
T1/2	1.8				1.2

时间/d	山东省				安徽省
	残留量/(mg/kg)			消解率/%	残留量/(mg/kg)			消解率/%
	噻虫嗪	噻虫胺	噻虫嗪总和	消解率/%	噻虫嗪	噻虫胺	噻虫嗪总和	消解率/%
0.083	3.13	<0.01	3.14		2.04	0.0146	2.05
1	2.13	0.132	2.28	27.2	1.51	0.173	1.72	16.3
2	1.38	0.121	1.52	51.5	0.499	0.0464	0.553	73.0
3	0.951	0.0926	1.06	66.3	0.326	0.0213	0.351	82.9
5	0.440	0.0470	0.495	84.2	0.135	0.0136	0.151	92.6
7	0.195	0.0298	0.230	92.7	0.0324	<0.01	0.0424	97.9
14	<0.01	<0.01	<0.02		<0.01	<0.01	<0.02
21	<0.01	<0.01	<0.02		<0.01	<0.01	<0.02
方程	C=3.28e^-0.3789^T				C=2.2209e^-0.5651^T
R²	0.9999				0.9813
T1/2	1.8				1.2

施药剂量/ (g a.i./hm²)	施药次数	采收间隔期	残留量/ (mg/kg)	残留中值 (STMR)	残留最大值(HR)
56.25~84.375	2~3	2 h	0.573, 0.584, 0.601, 0.646, 0.646, 0.679, 0.856, 0.859, 0.883, 0.951, 0.960, 0.999, 1.01, 1.04, 1.08, 1.15, 1.16, 1.2, 1.31, 1.33, 1.36, 1.38, 1.41, 1.41, 1.41, 1.43, 1.43, 1.54, 1.59, 1.60, 1.63, 1.69, 1.72, 1.94, 2.08, 2.08, 2.21, 2.25, 2.28, 2.29, 2.33, 2.33, 2.82, 2.83, 2.92, 2.99, 2.994, 3.06	1.41	3.06
		5 d	0.0665, 0.0834, 0.0887, 0.0954, 0.101, 0.101, 0.128, 0.131, 0.132, 0.137, 0.139, 0.139, 0.174, 0.177, 0.177, 0.181, 0.186, 0.193, 0.197, 0.219, 0.219, 0.223, 0.227, 0.233, 0.239, 0.240, 0.241, 0.248, 0.251, 0.265, 0.300, 0.305, 0.306, 0.313, 0.313, 0.313, 0.351, 0.354, 0.361, 0.366, 0.376, 0.396, 0.406, 0.407, 0.410, 0.469, 0.470, 0.475, 0.503, 0.522, 0.528, 0.538, 0.560, 0.569, 0.584, 0.590, 0.606, 0.759, 0.767, 0.767, 0.775, 0.802, 0.821, 0.912, 0.973, 0.988, 0.996, 1.11, 1.14, 1.25, 1.27, 1.27	0.332	1.27
		7 d	0.0396, 0.0415, 0.0415, 0.0423, 0.0426, 0.0440, 0.0457, 0.0465, 0.0499, 0.0508, 0.0525, 0.0562, 0.0576, 0.0598, 0.0607, 0.0627, 0.0676, 0.0687, 0.0687, 0.0703, 0.0722, 0.0723, 0.0816, 0.0829, 0.0858, 0.0868, 0.0918, 0.0928, 0.0935, 0.09370.0962, 0.0967, 0.0969, 0.0972, 0.0972, 0.0978, 0.106, 0.123, 0.123, 0.124, 0.141, 0.144, 0.145, 0.146, 0.146, 0.147, 0.147, 0.152, 0.156, 0.157, 0.161, 0.170, 0.182, 0.188, 0.190, 0.193, 0.205, 0.221, 0.226, 0.227, 0.232, 0.233, 0.24, 0.269, 0.271, 0.272, 0.359, 0.36, 0.361, 0.394, 0.398, 0.406	0.102	0.406
		10 d	<0.02(19), 0.0190, 0.0192, 0.0229, 0.0232, 0.0236, 0.0236, 0.0282, 0.0283, 0.0291, 0.0295, 0.0296, 0.0330, 0.0358, 0.0363, 0.0363, 0.0382, 0.0396, 0.0402, 0.0466, 0.0471, 0.0482, 0.0529, 0.0539, 0.0548, 0.0565, 0.0565, 0.0571, 0.0598, 0.0599, 0.0609, 0.0612, 0.0625, 0.0629, 0.0760, 0.0785, 0.0785, 0.0809, 0.0830, 0.0868, 0.0918, 0.0948, 0.0965, 0.108, 0.109, 0.109, 0.113, 0.113, 0.119, 0.123, 0.124, 0.129	0.0373	0.129

施药剂量/ (g a.i./hm²)	施药次数	采收间隔期	残留量/ (mg/kg)	残留中值 (STMR)	残留最大值(HR)
56.25~84.375	2~3	2 h	0.573, 0.584, 0.601, 0.646, 0.646, 0.679, 0.856, 0.859, 0.883, 0.951, 0.960, 0.999, 1.01, 1.04, 1.08, 1.15, 1.16, 1.2, 1.31, 1.33, 1.36, 1.38, 1.41, 1.41, 1.41, 1.43, 1.43, 1.54, 1.59, 1.60, 1.63, 1.69, 1.72, 1.94, 2.08, 2.08, 2.21, 2.25, 2.28, 2.29, 2.33, 2.33, 2.82, 2.83, 2.92, 2.99, 2.994, 3.06	1.41	3.06
		5 d	0.0665, 0.0834, 0.0887, 0.0954, 0.101, 0.101, 0.128, 0.131, 0.132, 0.137, 0.139, 0.139, 0.174, 0.177, 0.177, 0.181, 0.186, 0.193, 0.197, 0.219, 0.219, 0.223, 0.227, 0.233, 0.239, 0.240, 0.241, 0.248, 0.251, 0.265, 0.300, 0.305, 0.306, 0.313, 0.313, 0.313, 0.351, 0.354, 0.361, 0.366, 0.376, 0.396, 0.406, 0.407, 0.410, 0.469, 0.470, 0.475, 0.503, 0.522, 0.528, 0.538, 0.560, 0.569, 0.584, 0.590, 0.606, 0.759, 0.767, 0.767, 0.775, 0.802, 0.821, 0.912, 0.973, 0.988, 0.996, 1.11, 1.14, 1.25, 1.27, 1.27	0.332	1.27
		7 d	0.0396, 0.0415, 0.0415, 0.0423, 0.0426, 0.0440, 0.0457, 0.0465, 0.0499, 0.0508, 0.0525, 0.0562, 0.0576, 0.0598, 0.0607, 0.0627, 0.0676, 0.0687, 0.0687, 0.0703, 0.0722, 0.0723, 0.0816, 0.0829, 0.0858, 0.0868, 0.0918, 0.0928, 0.0935, 0.09370.0962, 0.0967, 0.0969, 0.0972, 0.0972, 0.0978, 0.106, 0.123, 0.123, 0.124, 0.141, 0.144, 0.145, 0.146, 0.146, 0.147, 0.147, 0.152, 0.156, 0.157, 0.161, 0.170, 0.182, 0.188, 0.190, 0.193, 0.205, 0.221, 0.226, 0.227, 0.232, 0.233, 0.24, 0.269, 0.271, 0.272, 0.359, 0.36, 0.361, 0.394, 0.398, 0.406	0.102	0.406
		10 d	<0.02(19), 0.0190, 0.0192, 0.0229, 0.0232, 0.0236, 0.0236, 0.0282, 0.0283, 0.0291, 0.0295, 0.0296, 0.0330, 0.0358, 0.0363, 0.0363, 0.0382, 0.0396, 0.0402, 0.0466, 0.0471, 0.0482, 0.0529, 0.0539, 0.0548, 0.0565, 0.0565, 0.0571, 0.0598, 0.0599, 0.0609, 0.0612, 0.0625, 0.0629, 0.0760, 0.0785, 0.0785, 0.0809, 0.0830, 0.0868, 0.0918, 0.0948, 0.0965, 0.108, 0.109, 0.109, 0.113, 0.113, 0.119, 0.123, 0.124, 0.129	0.0373	0.129