Residues and dietary risk assessment of fluopyram in Dendrobium officinale

doi:10.3969/j.issn.1004-1524.20230479

Acta Agriculturae Zhejiangensis ›› 2024, Vol. 36 ›› Issue (7): 1666-1676.DOI: 10.3969/j.issn.1004-1524.20230479

• Quality and Safety of Agricultural Products • Previous Articles Next Articles

Residues and dietary risk assessment of fluopyram in Dendrobium officinale

WANG Xiaomei¹^,²(), LUO Yuqin², ZHAO Xueping², LU Lanfei¹^,², FANG Nan², WANG Xiangyun², JIANG Jinhua², HE Hongmei², ZHANG Changpeng²^,^*(), WANG Qiang¹^,²^,^*()

1. College of Life Sciences, China Jiliang University, Hangzhou 310018, China
2. Institute of Agro-Products Safety and Nutrition, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China

Received:2023-04-11 Online:2024-07-25 Published:2024-08-05

Abstract

Abstract:

A method was established for the simultaneous determination of fluopyram and its metabolite 2-(trifluoromethyl) benzamide (BZM) in both fresh and dried Dendrobium officinale. Pot experiment was conducted to investigate the residue behaviors of fluopyram and BZM in D. officinale, and the long-term dietary risk of fluopyram was evaluated. The established determination method was as follows: the samples were extracted with acetonitrile, purified with octadecyl bonded silica gel (C₁₈), primary secondary amine (PSA) and PestiCarb (PC), and detected by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The result showed that fluopyram and BZM had linearities that ranged from 0.001 to 0.1 mg·L^-1, with correlation coefficient≥ 0.998 1. The recoveries of fluopyram and BZM in D. officinale at three spiked levels (0.01, 0.1, 15 mg·kg^-1) were 85.71%-97.98%, 94.14%-112.21%, respectively, with relative standard deviations of 0.39%-5.93%, 1.22%-6.73%, respectively. When fluopyram was applied at recommended does (375.3 g·hm^-2, based on the available ingredient) or double recommended does to D. officinale, the dissipation dynamics of fluopyram fitted the first-order kinetics equation, and the half-life of fluopyram in D. officinale was 19.20-28.76 d, indicating that fluopyram fell under the category of easily degradable pesticides. The residues of fluopyram and BZM in D. officinale did not exceed 1.98, 0.09 mg·kg^-1 after 75 days of application under the experiment contions. Calculation results showed that the national estimated daily intake of fluopyram was 0.380 6 mg for the general population under the given conditions, and the corresponding dietary risk quotient was 60.41%, which indicated that applying 41.7% fluopyram suspension concentrate (SC) at the recommended dosage on D. officinale would not pose an unacceptable risk to human health.

Key words: fluopyram, Dendrobium officinale, ultra-performance liquid chromatography-tandem mass spectrometry, pesticide residue, dietary risk assessment

CLC Number:

S481.8

WANG Xiaomei, LUO Yuqin, ZHAO Xueping, LU Lanfei, FANG Nan, WANG Xiangyun, JIANG Jinhua, HE Hongmei, ZHANG Changpeng, WANG Qiang. Residues and dietary risk assessment of fluopyram in Dendrobium officinale[J]. Acta Agriculturae Zhejiangensis, 2024, 36(7): 1666-1676.

Figures/Tables 11

References 35

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化合物 Compound	母离子 Precursor	子离子 Product	锥孔电压 Cone voltage/V	碰撞电压 Collision energy/V
氟吡菌酰胺Fluopyram	397.1	208.0	30	40
		173.0^*	30	30
2-(三氯甲基)苯甲酰胺	190.0	170.0^*	20	10
2-(Trifluoromethyl) benzamide		130.0	20	20

化合物 Compound	母离子 Precursor	子离子 Product	锥孔电压 Cone voltage/V	碰撞电压 Collision energy/V
氟吡菌酰胺Fluopyram	397.1	208.0	30	40
		173.0^*	30	30
2-(三氯甲基)苯甲酰胺	190.0	170.0^*	20	10
2-(Trifluoromethyl) benzamide		130.0	20	20

样品 Sample	化合物 Compound	线性范围 Linear range/ (mg·L^-1)	回归方程 Regression equation	决定系数 Determination coefficient	基质效应 Matrix effect	检出限 LOD/ (mg·L^-1)	定量限 LOQ/ (mg·kg^-1)
鲜茎	氟吡菌酰胺Fluopyram	0.001~0.1	y=4 250 459.188 1 x+3 037.381 8	0.998 1	0.93	0.001	0.001
Fresh stem	BZM	0.001~0.1	y=2 938 537.804 7 x+1 388.699 0	0.998 9	0.89	0.001	0.001
干茎	氟吡菌酰胺Fluopyram	0.001~0.1	y=1 834 865.947 1 x+394.743 1	1.000 0	0.89	0.01	0.01
Dried stem	BZM	0.001~0.1	y=1 062 565.961 4x-416.343 0	1.000 0	0.71	0.01	0.01

样品 Sample	化合物 Compound	线性范围 Linear range/ (mg·L^-1)	回归方程 Regression equation	决定系数 Determination coefficient	基质效应 Matrix effect	检出限 LOD/ (mg·L^-1)	定量限 LOQ/ (mg·kg^-1)
鲜茎	氟吡菌酰胺Fluopyram	0.001~0.1	y=4 250 459.188 1 x+3 037.381 8	0.998 1	0.93	0.001	0.001
Fresh stem	BZM	0.001~0.1	y=2 938 537.804 7 x+1 388.699 0	0.998 9	0.89	0.001	0.001
干茎	氟吡菌酰胺Fluopyram	0.001~0.1	y=1 834 865.947 1 x+394.743 1	1.000 0	0.89	0.01	0.01
Dried stem	BZM	0.001~0.1	y=1 062 565.961 4x-416.343 0	1.000 0	0.71	0.01	0.01

化合物 Compound	样品 Sample	添加水平 Spiking level/(mg·kg^-1)	回收率 Recovery/%	相对标准偏差 RSD/%
氟吡菌酰胺	鲜茎Fresh stem	0.001	85.71	5.93
Fluopyram		0.1	91.80	2.48
		15	88.10	3.62
	干茎Dried stem	0.01	93.27	0.39
		0.1	96.52	0.99
		15	97.98	2.72
BZM	鲜茎Fresh stem	0.001	94.14	6.73
		0.1	95.87	3.54
		15	107.88	2.87
	干茎Dried stem	0.01	98.88	4.31
		0.1	98.61	1.22
		15	112.21	1.93

Residues and dietary risk assessment of fluopyram in Dendrobium officinale

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样品 Sample	不同剂量下的回归方程 Regression equation under different doses		不同剂量下的半衰期 Half-life under different doses/d
样品 Sample	推荐剂量 Recommended dose	二倍推荐剂量 Double recommended does	推荐剂量 Recommended dose	二倍推荐剂量 Double recommended does
鲜茎Fresh stem	C_t=3.258 7e^{-0.036 1}^t(0.829 3)	C_t=5.126 8e^{-0.030 4}^t(0.849 4)	19.20	22.80
干茎Dried stem	C_t=7.7800e^{-0.028 2}^t(0.878 2)	C_t=9.482 2e^{-0.024 1}^t(0.908 3)	24.58	28.76

登记作物 Registration crop	食物种类 Food classification	膳食量 Dietary intake/kg	参考限量 Reference limit/(mg·kg^-1)	NEDI/mg
马铃薯Potato	薯类Tubers	0.049 5	0.03	0.001 5
辣椒Pepper	深色蔬菜Dark vegetables	0.091 5	2	0.183 0
黄瓜Cucumber	浅色蔬菜Light vegetables	0.183 7	0.5	0.091 9
葡萄Grape	水果Fruits	0.045 7	2	0.091 4
坚果Nuts	坚果Nuts	0.003 9	0.04	0.000 2
铁皮石斛Dendrobium officinale	酱油Soy sauce	0.009 0	1.41	0.012 7

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