Detection of 9 Fungicides Residues in Lychee Based on High-performance Liquid Chromatography-tandem Quadrupole-time of Flight-mass Spectrometry

doi:10.11924/j.issn.1000-6850.casb2024-0581

Abstract

Abstract:

The paper aims to scientifically evaluate the safety of nine fungicides on lychees. A method of the simultaneous detection for 9 fungicides in lychee was established by a high-performance liquid chromatography-tandem quadrupole-time of flight-mass spectrometry (HPLC-Q-TOF/MS). The QuEChERS pre-treatment salt package were firstly added in homogenized samples, and then extracted with acetonitrile. The automated QuEChERS sample processing platform was shaken for 10 minutes to remove impurities of lychee. The data were collected by HPLC-Q-TOF/MS. The calibration curves of 9 fungicides showed good linearity in a concentration range of 0.001-0.1 mg/L (R²>0.99). The average recoveries were 76.6%-114.8% at three spiked levels (0.005, 0.05, 0.1 mg/kg), while the relative standard deviations (RSD) were 1.4%-16.4%. The limits of detection and limits of quantification were 1 μg/kg and 3 μg/kg, respectively. The residue samples were analyzed by using the established detection method. The results showed that the residues of pyrazoxystrobin, azoxystrobin, difenoconazole, and metalaxyl in the whole lychee were all below the maximum residue limit values (MRLs) set by China. The established analytical method is reliable, simple and fast, and suitable for batch samples detection.

Key words: lychee, fungicides, high-performance liquid chromatography-tandem quadrupole-time of flight-mass spectrometry, pesticide residue, safe application, detection analysis

HU Fuchu, LIU Yanping, DUAN Yun, CHEN Tangzuan, ZHOU Wenjing, WANG Xianghe, WANG Siwei. Detection of 9 Fungicides Residues in Lychee Based on High-performance Liquid Chromatography-tandem Quadrupole-time of Flight-mass Spectrometry[J]. Chinese Agricultural Science Bulletin, 2025, 41(16): 143-149.

Figures/Tables 7

References 24

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农药商品名	农药有效成分	低浓度	高浓度
健达	21.2%氟唑菌酰胺、21.2%吡唑醚菌酯	3000倍	2000倍
凯润	25%吡唑醚菌酯	3000倍	2000倍
锐收果香	20%氯氟醚菌唑、20%吡唑醚菌酯	3000倍	2000倍
阿米妙收	200 g/L/嘧菌酯、125 g/L苯醚甲环唑	2000倍	1500倍
美甜	75 g/L氟唑菌酰羟胺、125 g/L苯醚甲环唑	2000倍	1500倍
宝路	11%咯菌腈、甲霜灵、嘧菌酯悬浮种衣剂	3000倍	2000倍
势克	25%苯醚甲环唑	3000倍	2000倍
德势	18.7%嘧菌酯、丙环唑	2000倍	1500倍

农药商品名	农药有效成分	低浓度	高浓度
健达	21.2%氟唑菌酰胺、21.2%吡唑醚菌酯	3000倍	2000倍
凯润	25%吡唑醚菌酯	3000倍	2000倍
锐收果香	20%氯氟醚菌唑、20%吡唑醚菌酯	3000倍	2000倍
阿米妙收	200 g/L/嘧菌酯、125 g/L苯醚甲环唑	2000倍	1500倍
美甜	75 g/L氟唑菌酰羟胺、125 g/L苯醚甲环唑	2000倍	1500倍
宝路	11%咯菌腈、甲霜灵、嘧菌酯悬浮种衣剂	3000倍	2000倍
势克	25%苯醚甲环唑	3000倍	2000倍
德势	18.7%嘧菌酯、丙环唑	2000倍	1500倍

杀菌剂	离子化模式	理论值	实测值(m/z)	误差(×10^-6)	二级碎片(m/z)
氟唑菌酰胺	5.02	ESI-	380.0828	380.0832	0.95
吡唑醚菌酯	7.67	ESI+	388.1059	388.1055	-1.08
氯氟醚菌唑	7.26	ESI+	398.0878	398.0879	0.25
苯醚甲环唑	10.82	ESI+	406.0720	406.0723	0.69
嘧菌酯	3.53	ESI+	404.1241	404.1245	0.99
氟唑菌酰羟胺	9.57	ESI+	426.0349	426.0355	1.41
咯菌腈	4.12	ESI-	247.0325	247.0331	2.43
甲霜灵	3.39	ESI+	280.1543	280.1542	-0.54
丙环唑	6.92	ESI+	342.0771	342.0776	1.46

杀菌剂	离子化模式	理论值	实测值(m/z)	误差(×10^-6)	二级碎片(m/z)
氟唑菌酰胺	5.02	ESI-	380.0828	380.0832	0.95
吡唑醚菌酯	7.67	ESI+	388.1059	388.1055	-1.08
氯氟醚菌唑	7.26	ESI+	398.0878	398.0879	0.25
苯醚甲环唑	10.82	ESI+	406.0720	406.0723	0.69
嘧菌酯	3.53	ESI+	404.1241	404.1245	0.99
氟唑菌酰羟胺	9.57	ESI+	426.0349	426.0355	1.41
咯菌腈	4.12	ESI-	247.0325	247.0331	2.43
甲霜灵	3.39	ESI+	280.1543	280.1542	-0.54
丙环唑	6.92	ESI+	342.0771	342.0776	1.46

杀菌剂		0.005 mg/kg				0.05 mg/kg			0.1 mg/kg
杀菌剂		平均回收率		相对标准偏差		平均回收率	相对标准偏差		平均回收率	相对标准偏差
氟唑菌酰胺	114.8		5.6		107.1		4.8	97.7		5.2
吡唑醚菌酯	116.4		7.2		107.7		5.39	101.6		8.5
氯氟醚菌唑	93.0		8.9		108.0		8.7	109.9		4.6
苯醚甲环唑	115.4		4.6		117.8		2.0	115.7		15.4
嘧菌酯	107.1		5.5		116.2		15.7	87.2		16.1
氟唑菌酰羟胺	113.3		1.4		117.1		7.6	110.9		4.6
咯菌腈	76.6		12.5		81.7		8.1	79.2		9.2
甲霜灵	88.0		16.4		90.5		14.0	78.8		13.0
丙环唑	93.0		8.6		91.0		6.9	87.4		8.1