Simultaneous detection and dietary exposure risk assessment of 16 pesticides in mudflat shellfish and mariculture environment

doi:10.3969/j.issn.1004-1524.20250371

Acta Agriculturae Zhejiangensis ›› 2026, Vol. 38 ›› Issue (4): 769-780.DOI: 10.3969/j.issn.1004-1524.20250371

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

Simultaneous detection and dietary exposure risk assessment of 16 pesticides in mudflat shellfish and mariculture environment

ZHU Jie¹^,²^,³^,⁴(), XU Huibin¹^,²^,³^,⁴, XIANG Linmin⁵, HU Yuan¹^,²^,³^,⁴, LU Rongmao¹^,²^,³^,⁴, CAI Jingbo¹^,²^,³^,⁴^,^*()

¹ Zhejiang Mariculture Research Institute, Wenzhou 325000, Zhejiang, China
² Zhejiang Key Laboratory of Coastal Biological Germplasm Resources Conservation and Utilization, Wenzhou 325000, Zhejiang, China
³ Sino-Thai Joint Laboratory of Marine Science and Technology, Wenzhou 325000, Zhejiang, China
⁴ Wenzhou Key Laboratory of Marine Biological Genetics and Breeding, Wenzhou 325000, Zhejiang, China
⁵ Wenzhou Quality and Technology Testing Research Institute, Wenzhou 325013, Zhejiang, China

Received:2025-05-12 Online:2026-04-25 Published:2026-05-08
Contact: CAI Jingbo

Abstract

Abstract:

To clarify the quality and safety status of coastal mudflat mariculture in Zhejiang Province of China, a sensitive analytical method was established for the simultaneous determination of 16 pesticide residues (including organophosphorus, pyrethroid, and macrolide pesticides) in aquatic products and their mariculture environment using dispersive solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry. Samples were extracted with 2% acetic acid in acetonitrile, and the extracts were purified using QuEChERS extraction salt packets and QuEChERS cleanup tubes prior to instrumental analysis. This method was applied to determine the residual levels of the 16 target pesticides in mudflat shellfish and their mariculture environment from typical mariculture areas in southern Zhejiang during 2024-2025, and a dietary exposure risk assessment was conducted for the detected pesticides. It was shown that the established method exhibited good linearity for all 16 pesticides in the concentration range of 1-50 ng·mL^-1, with coefficients of determination (R²) all exceeding 0.995. The recoveries at four spiked levels (4, 10, 20, and 50 μg·kg^-1) ranged from 65.21% to 120.00%, with relative standard deviations (RSDs) of 0.24%-11.17%. The limit of quantification (LOQ) of triazophos was 0.1 μg·kg^-1 in biological samples, 0.5 μg·kg^-1 in sediment samples, and 0.5 μg·L^-1 in water samples; for the other 15 target pesticides, the LOQs were 0.2-4.0 μg·kg^-1 in biological samples, 0.8-10.0 μg·kg^-1 in sediment samples, and 0.8-10.0 μg·L^-1 in water samples. By using the established method, triazophos and fenpropathrin residues were detected in shellfish samples, and triazophos residue was detected in sediment samples, while no pesticide residues were found in water samples. The chronic dietary risk of the two detected pesticides ranged from 0.007% to 0.578%, and the acute dietary risk ranged from 0.845% to 51.798%, all below 100%, indicating that the dietary exposure risks were within an acceptable range.

Key words: mudflat shellfish, pesticide residues, mariculture environment, monitor, dietary exposure, risk assessment

CLC Number:

S931.3

ZHU Jie, XU Huibin, XIANG Linmin, HU Yuan, LU Rongmao, CAI Jingbo. Simultaneous detection and dietary exposure risk assessment of 16 pesticides in mudflat shellfish and mariculture environment[J]. Acta Agriculturae Zhejiangensis, 2026, 38(4): 769-780.

Figures/Tables 10

References 35

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药剂 Reagent	母离子 Parent ion	子离子 Daughter ion	锥孔电压/V Cone voltage/V	碰撞能量/eV Collision energy/eV
甲胺磷Methamidophos	142.1	94.0^*/125.0	30	10/10
敌敌畏Dichlorvos	221.2	109.0^*/127.0	30	15/20
乐果Dimethoate	230.1	199.0^*/125.0	30	10/20
敌百虫Trichlorfon	257.1	109.0^*/221.0	30	18/10
对硫磷Parathion	292.2	236.0^*/264.0	30	15/10
辛硫磷Phoxim	299.0	129.0^*/153.0	30	15/5
三唑磷Triazophos	314.0	162.0^*/119.1	30	20/35
马拉硫磷Malathion	331.1	127.0^*/285.0	30	10/15
甲氰菊酯Fenpropathrin	350.3	125.2^*/97.2	20	15/25
氯菊酯Permethrin	408.5	183.1^*/355.2	20	20/5
氯氰菊酯Cypermethrin	433.1	191.0^*/127.0	30	10/30
氰戊菊酯Fenvalerate	437.2	167.0^*/208.0	20	20/10
氟氰戊菊酯Flucythrinate	469.2	412.2^*/199.2	20	10/16
溴氰菊酯Deltamethrin	523.2	280.9^*/506.0	20	15/10
阿维菌素Abamectin	895.5	751.5^*/449.0	30	40/50
伊维菌素Ivermectin	897.5	753.4^*/329.2	30	45/52

药剂 Reagent	母离子 Parent ion	子离子 Daughter ion	锥孔电压/V Cone voltage/V	碰撞能量/eV Collision energy/eV
甲胺磷Methamidophos	142.1	94.0^*/125.0	30	10/10
敌敌畏Dichlorvos	221.2	109.0^*/127.0	30	15/20
乐果Dimethoate	230.1	199.0^*/125.0	30	10/20
敌百虫Trichlorfon	257.1	109.0^*/221.0	30	18/10
对硫磷Parathion	292.2	236.0^*/264.0	30	15/10
辛硫磷Phoxim	299.0	129.0^*/153.0	30	15/5
三唑磷Triazophos	314.0	162.0^*/119.1	30	20/35
马拉硫磷Malathion	331.1	127.0^*/285.0	30	10/15
甲氰菊酯Fenpropathrin	350.3	125.2^*/97.2	20	15/25
氯菊酯Permethrin	408.5	183.1^*/355.2	20	20/5
氯氰菊酯Cypermethrin	433.1	191.0^*/127.0	30	10/30
氰戊菊酯Fenvalerate	437.2	167.0^*/208.0	20	20/10
氟氰戊菊酯Flucythrinate	469.2	412.2^*/199.2	20	10/16
溴氰菊酯Deltamethrin	523.2	280.9^*/506.0	20	15/10
阿维菌素Abamectin	895.5	751.5^*/449.0	30	40/50
伊维菌素Ivermectin	897.5	753.4^*/329.2	30	45/52

组别 Group	不同农药的提取率Extraction rate of different reagents
组别 Group	甲胺磷 Methamidophos	敌敌畏 Dichlorvos	乐果 Dimethoate	敌百虫 Trichlorfon	对硫磷 Parathion	辛硫磷 Phoxim	三唑磷 Triazophos	马拉硫磷 Malathion
G1	82.42±2.00 b	64.28±1.18 c	58.55±1.75 a	181.52±0.69 a	101.96±0.40 b	98.37±1.39 c	123.09±0.36 a	99.77±1.48 c
G2	89.69±6.44 ab	120.10±7.21 a	62.59±5.33 a	36.27±3.15 d	104.37±3.44 ab	104.86±1.09 ab	117.97±2.90 b	105.39±1.54 b
G3	94.02±3.38 a	106.88±2.18 b	65.47±3.54 a	67.35±3.55 b	107.05±1.72 a	103.66±1.15 b	122.45±0.10 a	109.31±0.83 a
G4	93.20±2.54 a	102.29±1.05 b	62.48±3.73 a	59.72±2.36 c	107.53±2.51 a	106.85±1.45 a	122.66±0.61 a	107.18±0.74 ab
G5	89.97±4.15 ab	115.21±2.52 a	62.48±4.44 a	34.66±3.68 d	105.52±2.24 ab	104.41±1.55 ab	118.63±1.89 b	104.65±2.78 b
组别 Group	不同农药的提取率Extraction rate of different reagents
组别 Group	甲氰菊酯 Fenpropathrin	氯菊酯 Permethrin	氯氰菊酯 Cypermethrin	氰戊菊酯 Fenvalerate	氟氰戊菊酯 Flucythrinate	溴氰菊酯 Deltamethrin	阿维菌素 Abamectin	伊维菌素 Ivermectin
G1	101.30±3.64 bc	85.14±8.01 a	101.075±7.31 a	98.39±7.42 ab	98.16±2.31 b	97.66±1.35 a	70.28±0.10 b	65.22±0.86 d
G2	104.61±4.66 ab	87.27±7.34 a	96.52±1.39 a	95.42±8.33 b	107.24±3.75 a	100.80±3.43 a	71.77±2.49 b	69.08±1.54 cd
G3	108.32±2.50 a	94.40±4.14 a	91.78±17.06 a	115.18±9.64 a	112.20±2.86 a	101.47±2.66 a	82.58±2.82 a	84.70±2.46 a
G4	105.38±2.19 ab	89.57±5.66 a	103.86±2.15 a	87.60±5.97 b	109.31±5.28 a	102.75±3.34 a	81.23±0.51 a	78.41±1.53 b
G5	96.93±1.75 c	83.74±3.30 a	101.86±4.63 a	102.41±10.14 ab	105.85±6.43 ab	99.93±0.91 a	72.58±1.32 b	70.18±7.49 c

组别 Group	不同农药的提取率Extraction rate of different reagents
组别 Group	甲胺磷 Methamidophos	敌敌畏 Dichlorvos	乐果 Dimethoate	敌百虫 Trichlorfon	对硫磷 Parathion	辛硫磷 Phoxim	三唑磷 Triazophos	马拉硫磷 Malathion
G1	82.42±2.00 b	64.28±1.18 c	58.55±1.75 a	181.52±0.69 a	101.96±0.40 b	98.37±1.39 c	123.09±0.36 a	99.77±1.48 c
G2	89.69±6.44 ab	120.10±7.21 a	62.59±5.33 a	36.27±3.15 d	104.37±3.44 ab	104.86±1.09 ab	117.97±2.90 b	105.39±1.54 b
G3	94.02±3.38 a	106.88±2.18 b	65.47±3.54 a	67.35±3.55 b	107.05±1.72 a	103.66±1.15 b	122.45±0.10 a	109.31±0.83 a
G4	93.20±2.54 a	102.29±1.05 b	62.48±3.73 a	59.72±2.36 c	107.53±2.51 a	106.85±1.45 a	122.66±0.61 a	107.18±0.74 ab
G5	89.97±4.15 ab	115.21±2.52 a	62.48±4.44 a	34.66±3.68 d	105.52±2.24 ab	104.41±1.55 ab	118.63±1.89 b	104.65±2.78 b
组别 Group	不同农药的提取率Extraction rate of different reagents
组别 Group	甲氰菊酯 Fenpropathrin	氯菊酯 Permethrin	氯氰菊酯 Cypermethrin	氰戊菊酯 Fenvalerate	氟氰戊菊酯 Flucythrinate	溴氰菊酯 Deltamethrin	阿维菌素 Abamectin	伊维菌素 Ivermectin
G1	101.30±3.64 bc	85.14±8.01 a	101.075±7.31 a	98.39±7.42 ab	98.16±2.31 b	97.66±1.35 a	70.28±0.10 b	65.22±0.86 d
G2	104.61±4.66 ab	87.27±7.34 a	96.52±1.39 a	95.42±8.33 b	107.24±3.75 a	100.80±3.43 a	71.77±2.49 b	69.08±1.54 cd
G3	108.32±2.50 a	94.40±4.14 a	91.78±17.06 a	115.18±9.64 a	112.20±2.86 a	101.47±2.66 a	82.58±2.82 a	84.70±2.46 a
G4	105.38±2.19 ab	89.57±5.66 a	103.86±2.15 a	87.60±5.97 b	109.31±5.28 a	102.75±3.34 a	81.23±0.51 a	78.41±1.53 b
G5	96.93±1.75 c	83.74±3.30 a	101.86±4.63 a	102.41±10.14 ab	105.85±6.43 ab	99.93±0.91 a	72.58±1.32 b	70.18±7.49 c

组别 Group	不同农药的提取率Extraction rate of different reagents
组别 Group	甲胺磷 Methamidophos	敌敌畏 Dichlorvos	乐果 Dimethoate	敌百虫 Trichlorfon	对硫磷 Parathion	辛硫磷 Phoxim	三唑磷 Triazophos	马拉硫磷 Malathion
G1	85.20±2.01 a	60.55±1.88 d	58.44±0.11 b	154.88±4.93 a	102.71±2.86 c	100.41±2.33 b	121.31±2.87 ab	99.33±1.44 c
G2	87.07±2.64 a	121.47±2.01 a	63.76±0.55 a	28.50±3.35 c	105.34±1.57 bc	104.18±2.15 a	118.61±0.49 b	103.97±1.35 b
G3	87.50±6.22 a	105.88±2.21 c	63.63±0.81 a	58.32±1.87 b	110.27±1.93 a	105.69±1.43 a	124.63±1.40 a	107.45±2.85 a
G4	90.68±1.29 a	102.86±2.07 c	60.15±1.69 b	52.55±1.47 b	106.65±1.05 ab	105.07±0.44 a	121.75±1.90 ab	104.97±0.85 ab
G5	85.94±5.17 a	115.52±3.70 b	63.17±0.56 a	30.85±1.68 c	105.63±1.70 bc	104.93±1.17 a	120.35±1.71 b	102.28±0.58 bc
组别 Group	不同农药的提取率Extraction rate of different reagents
组别 Group	甲氰菊酯 Fenpropathrin	氯菊酯 Permethrin	氯氰菊酯 Cypermethrin	氰戊菊酯 Fenvalerate	氟氰戊菊酯 Flucythrinate	溴氰菊酯 Deltamethrin	阿维菌素 Abamectin	伊维菌素 Ivermectin
G1	97.48±3.99 b	78.24±8.80 a	96.42±2.54 bc	99.02±2.19 ab	100.64±3.85 c	98.54±0.87 ab	67.92±4.18 b	55.93±1.04 b
G2	101.75±1.09 ab	78.62±2.70 a	90.66±5.37 c	84.80±13.26 b	110.30±3.34 a	102.26±1.63 a	65.82±2.16 b	56.16±2.56 b
G3	106.15±4.02 a	76.51±8.01 a	107.39±7.41 a	116.93±9.68 a	113.31±2.50 a	98.80±2.15 ab	82.32±3.59 a	60.91±1.97 a
G4	101.30±1.00 ab	79.70±1.80 a	103.15±2.76 ab	94.58±8.15 ab	107.56±2.58 ab	99.92±2.47 ab	78.07±1.86 a	55.57±0.38 b
G5	98.43±4.05 b	74.02±3.04 a	101.10±4.73 ab	83.87±21.82 b	103.42±4.44 bc	97.63±2.96 b	67.63±3.11 b	52.62±2.09 b

Simultaneous detection and dietary exposure risk assessment of 16 pesticides in mudflat shellfish and mariculture environment

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药剂 Reagent	在不同样本中的基质因子Matrix factor in different samples
药剂 Reagent	缢蛏 Sinonovacula constricta	泥蚶 Mud clam	彩虹明樱蛤 Moerella iridescens	海水 Sea water	沉积物 Sediment
甲胺磷Methamidophos	1.09	1.16	0.78	1.05	0.80
敌敌畏Dichlorvos	1.07	1.15	0.67	1.05	0.85
乐果Dimethoate	0.65	0.71	0.41	0.65	0.46
敌百虫Trichlorfon	0.70	0.74	0.46	0.70	0.51
对硫磷Parathion	1.04	1.06	0.68	1.04	0.77
辛硫磷Phoxim	0.92	1.01	0.74	1.01	0.77
三唑磷Triazophos	1.01	1.04	0.88	1.03	0.87
马拉硫磷Malathion	0.99	1.03	0.75	1.02	0.82
甲氰菊酯Fenpropathrin	0.90	0.99	0.64	1.01	0.86
氯菊酯Permethrin	0.68	0.79	0.60	0.92	0.84
氯氰菊酯Cypermethrin	1.06	1.05	0.86	1.01	0.91
氰戊菊酯Fenvalerate	0.87	0.85	0.59	0.92	0.79
氟氰戊菊酯Flucythrinate	1.12	1.10	0.74	1.03	0.83
溴氰菊酯Deltamethrin	0.95	0.98	0.65	1.00	0.88
阿维菌素Abamectin	1.42	1.20	1.33	0.96	1.02
伊维菌素Ivermectin	1.17	1.18	1.03	1.08	1.04

药剂 Reagent	在不同样品中的LOD LOD in different samples			在不同样品中的LOQ LOQ in different samples
药剂 Reagent	贝类/ (μg·kg^-1) Shellfish/ (μg·kg^-1)	沉积物/ (μg·kg^-1) Sediment/ (μg·kg^-1)	海水/ (μg·L^-1) Sea water/ (μg·L^-1)	贝类/ (μg·kg^-1) Shellfish/ (μg·kg^-1)	沉积物/ (μg·kg^-1) Sediment/ (μg·kg^-1)	海水/ (μg·L¹) Sea water/ (μg·L¹)
甲胺磷Methamidophos	1.0	1.0	1.5	3.0	4.0	4.5
敌敌畏Dichlorvos	1.0	1.0	1.5	3.0	4.0	4.5
乐果Dimethoate	1.0	1.0	1.0	3.0	3.0	3.0
敌百虫Trichlorfon	1.0	1.0	1.0	3.0	3.0	3.0
对硫磷Parathion	1.3	1.3	1.3	4.0	4.0	4.0
辛硫磷Phoxim	0.8	0.8	0.8	2.5	2.5	2.5
三唑磷Triazophos	0.033	0.15	0.15	0.1	0.5	0.5
马拉硫磷Malathion	0.05	0.25	0.3	0.2	0.8	0.8
甲氰菊酯Fenpropathrin	1.2	2.0	3.0	4.0	6.0	10.0
氯菊酯Permethrin	1.2	3.2	3.5	4.0	10.0	10.0
氯氰菊酯Cypermethrin	2.0	2.5	2.0	4.0	7.5	6.0
氰戊菊酯Fenvalerate	2.0	3.3	3.4	4.0	10.0	10.0
氟氰戊菊酯Flucythrinate	1.2	3.1	3.5	4.0	10.0	10.0
溴氰菊酯Deltamethrin	1.2	3.0	3.0	4.0	10.0	10.0
阿维菌素Abamectin	1.0	1.0	1.0	3.0	3.0	3.0
伊维菌素Ivermectin	1.0	1.0	1.0	3.0	3.0	3.0

药剂 Reagent	添加浓度/ (μg·kg^-1) Spiked dose/ (μg·kg^-1)	不同样品中的回收率/% Recovery rate in different samples/%			药剂 Reagent	添加浓度/ (μg·kg^-1) Spiked dose/ (μg·kg^-1)	不同样品中的回收率/% Recovery rate in different samples/%
药剂 Reagent	添加浓度/ (μg·kg^-1) Spiked dose/ (μg·kg^-1)	贝类 Shellfish	海水 Sea water	沉积物 Sediment	药剂 Reagent	添加浓度/ (μg·kg^-1) Spiked dose/ (μg·kg^-1)	贝类 Shellfish	海水 Sea water	沉积物 Sediment
甲胺磷	4	87.88±3.12	—	—	甲氰菊酯	4	98.75±5.29	—	—
Methamidophos	10	80.47±9.11	87.00±10.25	78.87±5.26	Fenpropathrin	10	98.73±4.49	100.38±4.46	106.87±4.62
	20	73.09±5.63	76.17±4.18	82.25±4.05		20	103.46±5.43	104.11±0.82	105.05±1.26
	50	83.27±1.38	81.11±3.06	80.92±3.19		50	107.46±1.54	102.56±1.62	103.86±1.73
敌敌畏	4	65.21±2.24	—	—	氯菊酯	4	81.63±1.47	—	—
Dichlorvos	10	69.28±7.22	99.67±2.36	88.98±4.36	Permethrin	10	96.17±9.27	107.88±10.15	115.58±2.53
	20	73.31±4.98	95.57±0.85	92.59±2.11		20	88.50±4.89	102.61±3.53	89.53±5.46
	50	85.68±3.80	96.79±0.83	94.37±1.72		50	103.16±4.94	105.87±5.97	107.08±2.27
乐果	4	104.13±1.01	—	—	氯氰菊酯	4	97.04±1.34	—	—
Dimethoate	10	102.50±4.54	103.93±1.72	93.23±1.02	Cypermethrin	10	98.63±5.17	104.95±5.76	106.80±6.96
	20	102.48±2.95	99.51±1.98	93.85±3.25		20	111.79±0.50	105.14±3.90	99.44±9.86
	50	105.65±4.48	98.92±2.29	97.86±4.38		50	115.74±3.17	105.26±3.42	100.24±0.43
敌百虫	4	103.17±1.37	—	—	氰戊菊酯	4	68.82±4.03	—	—
Trichlorfon	10	100.05±3.84	96.67±1.93	88.01±1.43	Fenvalerate	10	75.65±0.64	100.57±7.52	84.02±3.17
	20	97.10±4.39	93.26±2.76	88.72±3.34		20	101.88±0.74	91.68±6.93	84.02±7.34
	50	100.82±3.13	93.10±3.15	91.99±3.55		50	100.71±11.17	89.15±2.45	102.70±6.92
对硫磷	4	106.25±1.74	—	—	氟氰戊菊酯	4	73.42±3.71	—	—
Parathion	10	111.50±2.82	114.43±1.41	108.88±0.25	Flucythrinate	10	101.02±5.99	100.17±7.57	96.97±4.07
	20	100.75±0.66	106.58±0.75	105.70±3.50		20	100.42±8.40	98.66±2.71	107.01±1.53
	50	108.30±3.43	104.95±0.43	103.64±1.65		50	113.51±2.32	103.33±3.60	105.62±2.12
辛硫磷	4	103.50±1.41	—	—	溴氰菊酯	4	96.96±1.98	—	—
Phoxim	10	99.67±2.58	106.63±1.95	100.08±3.94	Deltamethrin	10	93.53±3.94	107.80±3.17	100.07±1.74
	20	101.31±2.64	103.31±0.99	102.15±0.49		20	104.17±1.59	100.98±2.37	100.22±9.94
	50	106.10±1.58	104.93±0.24	105.11±1.81		50	107.06±2.19	103.92±1.81	94.49±0.56
三唑磷	4	104.46±1.83	—	—	阿维菌素	4	97.50±4.02	—	—
Triazophos	10	113.32±2.92	110.63±1.10	102.27±2.92	Abamectin	10	90.92±5.64	98.18±3.15	89.88±6.11
	20	120.00±2.28	112.18±0.37	108.58±0.97		20	96.11±5.03	90.52±1.31	85.00±6.04
	50	118.87±0.98	115.71±0.28	112.22±1.18		50	97.34±2.14	96.05±2.51	88.98±2.63
马拉硫磷	4	94.79±3.43	—	—	伊维菌素	4	95.46±3.89	—	—
Malathion	10	96.08±0.74	107.48±1.94	98.58±2.81	Ivermectin	10	86.25±6.11	88.68±1.15	80.00±1.95
	20	100.06±2.96	105.28±1.16	103.34±0.94		20	89.76±3.47	88.78±0.77	83.13±2.71
	50	107.97±1.29	107.05±0.45	105.12±1.42		50	90.34±0.87	91.84±0.56	87.15±2.20

人群 Population	(C/m)/ (g·d^-1· kg^-1)	急性风险/% Acute risk/%
人群 Population	(C/m)/ (g·d^-1· kg^-1)	甲氰菊酯 Fenpropathrin	三唑磷 Triazophos
全部All	3.623 2	1.363	15.355
0~35月龄0-35 months	2.247 2	0.845	9.524
3~5岁3-5 years old	12.222 2	4.597	51.798
6~14岁6-14 years old	5.583 1	2.100	23.661
15~49岁15-49 years old	3.182 9	1.197	13.489
50~74岁50-74 years old	2.445 0	0.920	10.362
≥75岁≥75 years old	2.247 2	0.845	9.524

人群 Population	每日平均消费量/(g·d^-1) Daily consumption/(g·d^-1)	慢性风险/% Chronic risk/%
人群 Population	每日平均消费量/(g·d^-1) Daily consumption/(g·d^-1)	甲氰菊酯Fenpropathrin	三唑磷Triazophos
全部All	0.958 0	0.007	0.025
0~35月龄0-35 months	1.336 2	0.009	0.035
3~5岁3-5 years old	2.522 2	0.017	0.066
6~14岁6-14 years old	1.692 6	0.054	0.207
15~49岁15-49 years old	0.864 0	0.096	0.370
50~74岁50-74 years old	0.709 4	0.119	0.459
≥75岁≥75 years old	0.826 1	0.150	0.578

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t/min	流动相A的体积分数/% Volumn fraction of mobile phase A/%	流动相B的体积分数/% Volumn fraction of mobile phase B/%
0	3	97
1.0	3	97
1.5	15	85
2.5	50	50
7.0	70	30
9.0	98	2
13.0	98	2
13.1	3	97
15.0	3	97

t/min	流动相A的体积分数/% Volumn fraction of mobile phase A/%	流动相B的体积分数/% Volumn fraction of mobile phase B/%
0	3	97
1.0	3	97
1.5	15	85
2.5	50	50
7.0	70	30
9.0	98	2
13.0	98	2
13.1	3	97
15.0	3	97

组别 Group	不同农药的提取率Extraction rate of different reagents
组别 Group	甲胺磷 Methamidophos	敌敌畏 Dichlorvos	乐果 Dimethoate	敌百虫 Trichlorfon	对硫磷 Parathion	辛硫磷 Phoxim	三唑磷 Triazophos	马拉硫磷 Malathion
G1	90.98±5.17 b	74.17±5.77 b	61.24±3.74 b	126.60±2.59 a	115.11±8.49 a	108.38±7.47 b	114.23±9.02 a	111.46±8.22 b
G2	107.15±5.39 a	117.97±2.02 a	64.50±1.03 ab	58.32±2.18 c	119.01±1.67 a	117.54±0.79 a	119.65±1.15 a	119.67±1.69 ab
G3	92.09±5.53 b	115.26±3.00 a	63.82±2.40 b	63.04±1.94 b	118.84±3.41 a	113.31±4.81 ab	120.93±3.88 a	118.21±2.31 ab
G4	94.19±8.15 b	121.01±1.42 a	68.63±1.06 a	63.14±0.49 b	122.38±1.47 a	117.37±1.30 a	123.46±0.74 a	121.15±1.86 a
G5	93.81±3.73 b	121.23±1.62 a	64.04±1.42 b	51.05±2.95 d	118.98±1.23 a	118.08±1.19 a	121.56±2.12 a	119.90±1.86 ab
组别 Group	不同农药的提取率Extraction rate of different reagents
组别 Group	甲氰菊酯 Fenpropathrin	氯菊酯 Permethrin	氯氰菊酯 Cypermethrin	氰戊菊酯 Fenvalerate	氟氰戊菊酯 Flucythrinate	溴氰菊酯 Deltamethrin	阿维菌素 Abamectin	伊维菌素 Ivermectin
G1	105.92±6.68 b	105.96±7.21 a	106.89±6.23 b	110.22±5.31 ab	109.05±13.64 a	108.04±9.74 a	83.47±2.67 c	82.40±4.81 b
G2	115.91±0.32 a	107.48±3.84 a	119.57±3.85 a	103.72±4.13 b	117.77±5.10 a	111.96±1.13 a	NOTE	NOTE
G3	114.29±2.59 a	100.38±1.62 a	114.45±1.45 ab	107.84±6.59 ab	112.76±2.97 a	109.42±3.61 a	101.95±5.05 a	106.19±6.69 a
G4	120.03±3.19 a	110.91±5.17 a	117.18±4.94 a	122.15±10.93 a	117.75±9.80 a	115.95±2.75 a	100.76±1.27 a	103.01±3.83 a
G5	114.63±2.90 a	103.69±5.27 a	114.04±3.98 ab	122.59±9.35 a	112.93±6.99 a	115.67±1.66 a	91.25±3.87 b	89.65±3.83 b

组别 Group	不同农药的提取率Extraction rate of different reagents
组别 Group	甲胺磷 Methamidophos	敌敌畏 Dichlorvos	乐果 Dimethoate	敌百虫 Trichlorfon	对硫磷 Parathion	辛硫磷 Phoxim	三唑磷 Triazophos	马拉硫磷 Malathion
G1	90.98±5.17 b	74.17±5.77 b	61.24±3.74 b	126.60±2.59 a	115.11±8.49 a	108.38±7.47 b	114.23±9.02 a	111.46±8.22 b
G2	107.15±5.39 a	117.97±2.02 a	64.50±1.03 ab	58.32±2.18 c	119.01±1.67 a	117.54±0.79 a	119.65±1.15 a	119.67±1.69 ab
G3	92.09±5.53 b	115.26±3.00 a	63.82±2.40 b	63.04±1.94 b	118.84±3.41 a	113.31±4.81 ab	120.93±3.88 a	118.21±2.31 ab
G4	94.19±8.15 b	121.01±1.42 a	68.63±1.06 a	63.14±0.49 b	122.38±1.47 a	117.37±1.30 a	123.46±0.74 a	121.15±1.86 a
G5	93.81±3.73 b	121.23±1.62 a	64.04±1.42 b	51.05±2.95 d	118.98±1.23 a	118.08±1.19 a	121.56±2.12 a	119.90±1.86 ab
组别 Group	不同农药的提取率Extraction rate of different reagents
组别 Group	甲氰菊酯 Fenpropathrin	氯菊酯 Permethrin	氯氰菊酯 Cypermethrin	氰戊菊酯 Fenvalerate	氟氰戊菊酯 Flucythrinate	溴氰菊酯 Deltamethrin	阿维菌素 Abamectin	伊维菌素 Ivermectin
G1	105.92±6.68 b	105.96±7.21 a	106.89±6.23 b	110.22±5.31 ab	109.05±13.64 a	108.04±9.74 a	83.47±2.67 c	82.40±4.81 b
G2	115.91±0.32 a	107.48±3.84 a	119.57±3.85 a	103.72±4.13 b	117.77±5.10 a	111.96±1.13 a	NOTE	NOTE
G3	114.29±2.59 a	100.38±1.62 a	114.45±1.45 ab	107.84±6.59 ab	112.76±2.97 a	109.42±3.61 a	101.95±5.05 a	106.19±6.69 a
G4	120.03±3.19 a	110.91±5.17 a	117.18±4.94 a	122.15±10.93 a	117.75±9.80 a	115.95±2.75 a	100.76±1.27 a	103.01±3.83 a
G5	114.63±2.90 a	103.69±5.27 a	114.04±3.98 ab	122.59±9.35 a	112.93±6.99 a	115.67±1.66 a	91.25±3.87 b	89.65±3.83 b