氟吡菌酰胺在铁皮石斛中的残留与膳食风险

doi:10.3969/j.issn.1004-1524.20230479

浙江农业学报 ›› 2024, Vol. 36 ›› Issue (7): 1666-1676.DOI: 10.3969/j.issn.1004-1524.20230479

氟吡菌酰胺在铁皮石斛中的残留与膳食风险

王晓梅¹^,²(), 骆玉琴², 赵学平², 陆兰菲¹^,², 方楠², 王祥云², 蒋金花², 何红梅², 张昌朋²^,^*(), 王强¹^,²^,^*()

1.中国计量大学生命科学学院,浙江杭州 310018
2.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

收稿日期:2023-04-11 出版日期:2024-07-25 发布日期:2024-08-05
作者简介:王晓梅(1998—),女,河南平顶山人,硕士研究生,研究方向为农产品质量安全。E-mail: xiaomeiwang1019@163.com
通讯作者: *张昌朋,E-mail: cpzhang1215@zaas.ac.cn;王强,E-mail: wq13575733860@126.com
基金资助:
浙江省基础公益研究计划(LGN21C140006);浙江省农业标准化生产示范创建(“一县一品一策”)项目(ZJNY2022001-014)

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

摘要/Abstract

摘要：

建立一种可同时检测氟吡菌酰胺及其代谢物2-(三氯甲基)苯甲酰胺(BZM)在铁皮石斛(鲜样和干样)中残留量的分析方法,采用盆栽实验探究氟吡菌酰胺和BZM在铁皮石斛上的残留行为,评估氟吡菌酰胺的长期膳食风险。建立的检测方法为样品经乙腈提取后,用十八烷基硅烷键合硅胶、N-丙基乙二胺和石墨化碳净化,之后用超高效液相色谱-串联质谱法进行检测。在0.001~0.1 mg·L^-1范围内,所建立的氟吡菌酰胺和BZM检测方法线性关系良好,决定系数(R²)≥0.998 1。在0.01、0.1、15 mg·kg^-1的添加水平下,氟吡菌酰胺和BZM在铁皮石斛中的回收率分别为85.71%~97.98%、94.14%~112.21%,相对标准偏差分别为0.39%~5.93%、1.22%~6.73%。41.7%的氟吡菌酰胺悬浮剂以推荐剂量(有效成分375.3 g·hm^-2)或2倍推荐剂量施用1次,氟吡菌酰胺在铁皮石斛鲜茎和干茎上的消解均符合一级动力学方程,消解半衰期为19.20~28.76 d,属于易降解农药。在实验条件下,施药后75 d,氟吡菌酰胺和BZM在铁皮石斛中的残留量分别不超过1.98、0.09 mg·kg^-1。经测算,氟吡菌酰胺的全膳食国家估算每日摄入量为0.380 6 mg,对应的风险商为60.41%,说明41.7%的氟吡菌酰胺悬浮剂在推荐剂量下施用于铁皮石斛上并不会对人体健康产生不可接受的风险。

关键词: 氟吡菌酰胺, 铁皮石斛, 超高效液相色谱-串联质谱, 农药残留, 膳食风险评估

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

中图分类号:

S481.8

王晓梅, 骆玉琴, 赵学平, 陆兰菲, 方楠, 王祥云, 蒋金花, 何红梅, 张昌朋, 王强. 氟吡菌酰胺在铁皮石斛中的残留与膳食风险[J]. 浙江农业学报, 2024, 36(7): 1666-1676.

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.

图/表 11

图1 氟吡菌酰胺(A)及其代谢物2-(三氯甲基)苯甲酰胺的(B)结构示意图

Fig.1 The chemical structures of fluopyram (A) and its metabolite 2-(trifluoromethyl) benzamide (B)

表1 氟吡菌酰胺和2-(三氯甲基)苯甲酰胺的部分参数

Table 1 Parameters of fluopyram and 2-(trifluoromethyl) benzamide

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

图2 0.01 mg·L-1的氟吡菌酰胺(左)、2-(三氯甲基)苯甲酰胺(右)的多重反应监测色谱图

Fig.2 Multi-reaction monitoring chromatogram of 0.01 mg·L-1 fluopyram (left) and 2-(trifluoromethyl) benzamide (right)

图3 不同提取溶剂对铁皮石斛鲜样(A)和干样(B)中氟吡菌酰胺、2-(三氯甲基)苯甲酰胺(BZM)回收率的影响 S1、S2、S3、S4分别表示以乙腈、1%甲酸乙腈、甲醇、乙酸乙酯作为提取溶剂。

Fig.3 Effect of different extraction solvents on the recovery of fluopyram and 2-(trifluoromethyl) benzamide in fresh (A) and dried (B) Dendrobium officinale Extract solvents of S1, S2, S3, and S4 are acetonitrile, 1% formic acid acetonitrile, methanol, and ethyl acetate, respectively.

图4 石墨化碳(PC)添加量对铁皮石斛鲜样(A)和干样(B)中氟吡菌酰胺、2-(三氯甲基)苯甲酰胺(BZM)回收率的影响

Fig.4 Effect of application amount of PestiCarb (PC) on the recovery of fluopyram and 2-(trifluoromethyl) benzamide (BZM) in fresh (A) and dried (B) Dendrobium officinale

表2 氟吡菌酰胺和2-(三氯甲基)苯甲酰胺(BZM)的线性范围、回归方程、决定系数、基质效应、检出限和定量限

Table 2 Linear range, regression equation, determination coefficient, matrix effect, limit of detection (LOD) and limit of quantitation (LOQ) for fluopyram and 2-(trifluoromethyl) benzamide (BZM)

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

表3 氟吡菌酰胺和2-(三氯甲基)苯甲酰胺(BZM)在铁皮石斛上的回收率与相对标准偏差

Table 3 Recovery and relative standard deviation (RSD) of fluopyram and 2-(trifluoromethyl) benzamide (BZM) in Dendrobium officinale

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

图5 氟吡菌酰胺在铁皮石斛鲜样(A)和干样(B)中的消解动态

Fig.5 Decline dynamics of fluopyram in fresh (A) and dried (B) Dendrobium officinale

表4 氟吡菌酰胺在铁皮石斛鲜样和干样中的降解方程与半衰期

Table 4 Dynamics equation and half-life of fluopyram in fresh and dried Dendrobium officinale

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

图6 2-(三氯甲基)苯甲酰胺(BZM)在铁皮石斛鲜样(A)和干样(B)上的残留量

Fig.6 Residues of 2-(trifluoromethyl) benzamide in fresh (A) and dried (B) Dendrobium officinale

表5 推荐剂量氟吡菌酰胺在铁皮石斛中的长期膳食风险评估

Table 5 The chronic dietary risk assessment of fluopyram in Dendrobium officinale at recommended does

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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氟吡菌酰胺在铁皮石斛中的残留与膳食风险

Residues and dietary risk assessment of fluopyram in Dendrobium officinale

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