Evaluation of Graphene for Dispersive Solid-Phase Extraction of Triazine
               and Neonicotine Pesticides from Environmental Water

Wu, Xiao Li; Meng, Lixuan; Wu, Yanhua; Luk, Yan-Yeung; Ma, Yongqiang; Du, Yanli

doi:10.5935/0103-5053.20140227

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Articles • J. Braz. Chem. Soc. 26 (1) • Jan 2015 • https://doi.org/10.5935/0103-5053.20140227 copy

Evaluation of Graphene for Dispersive Solid-Phase Extraction of Triazine and Neonicotine Pesticides from Environmental Water

Authorship SCIMAGO INSTITUTIONS RANKINGS

In this work, graphene was used for dispersive solid-phase extraction of 11 triazine herbicides and 5 neonicotine insecticides from water. The extraction conditions such as the amount of graphene, the desorption solvent and the solution pH were optimized. Under the optimal conditions, high efﬁcient enrichment was achieved for the quantitative analysis of the pesticides. Triazines and neonicotines were determined by gas chromatograph-mass spectrometer (GC-MS) and high performance liquid chromatography electrospray tandem mass spectrometry (LC-MS/MS), respectively. The results indicated that graphene was an excellent adsorbent for the adsorption of pesticides. The recoveries of the pesticides were 83.0-108.9% with relative standard deviation (RSD) between 2.4% and 12.3%. The limits of detection (LODs) ranged from 0.03 μg L^-1 to 0.40 μg L^-1. Finally, the proposed method was applied for real sample analysis, such as tap and river water.

graphene; triazines; neonicotines; fast extraction

No.	Analyte	time / min	Parent ion / (m/z)	Product ion / (m/z)
1	Thiamethoxam	1.61	292	211^a a Quantitative ion. , 181
2	Imidacloprid	2.85	256	209, 175^a a Quantitative ion.
3	Imidaclothiz	3.49	262	181^a a Quantitative ion. , 122
4	Acetamiprid	4.30	223	126^a a Quantitative ion. , 56
5	Thiacloprid	7.32	253	186, 126^a a Quantitative ion.

No.	Analyte	time / min	Parent ion / (m/z)		Product ion / (m/z)
1	Prometon	8.73	210	225	168
2	Atrazine	8.90	200	215	202
3	Propazine	8.91	214	229	172
4	Terbuthylazine	9.11	214	229	173
5	Cyprazine	10.16	212	227	170
6	Metribuzin	10.20	198	144	214
7	Ametryn	10.44	227	170	212
8	Prometryn	11.47	241	184	68
9	Cyanazine	12.58	225	168	112
10	Procyazine	12.59	237	252	210
11	Hexazinone	14.68	171	128	252
12	TPP	14.74	326	325	215

Condition	Neonicotines	Triazines
Amount of graphene / mL	4, 5, 6^a a The optimal condition. , 7, 8	1, 2, 3^a a The optimal condition. , 4, 5
Desorption solvent	acetonitrile,^a a The optimal condition. ethyl acetate, acetone, methanol	acetonitrile,^a a The optimal condition. ethyl acetate. n-hexane, benzene
Desorption solvent volume / mL	4, 6, 7, 8^a a The optimal condition. , 10	6, 8^a a The optimal condition. , 10, 12, 14
pH of the solution	4, 6, 7^a a The optimal condition. , 8, 10	3, 5, 7^a a The optimal condition. , 9, 11

Analyte	Linear range / (μg L^-1)	R²	LOD / (μg L^-1)	LOQ /(μg L^-1)
Acetamiprid	0.5-100	0.9995	0.10	0.33
Imidacloprid	0.5-100	0.9998	0.05	0.17
Thiamethoxam	0.5-100	0.9993	0.15	0.50
Imidaclothiz	0.5-100	0.9995	0.05	0.17
Thiacloprid	0.5-100	0.9996	0.03	0.10
Prometon	0.5-100	0.9997	0.09	0.30
Atrazine	0.5-100	0.9997	0.12	0.40
Propazine	0.5-100	0.9993	0.15	0.50
Terbuthylazine	0.5-100	0.9996	0.04	0.13
Cyprazine	0.5-100	0.9987	0.25	0.83
Metribuzin	0.5-100	0.9979	0.23	0.77
Ametryn	0.5-100	0.999	0.12	0.40
Prometryn	0.5-100	0.9994	0.09	0.30
Cyanazine	0.5-100	0.9986	0.36	1.20
Procyazine	0.5-100	0.9995	0.40	1.30
Hexazinone	0.5-100	0.9992	0.26	0.87

Analyte	Spiked level / (μg L^-1)	Recovery / %	RSD / %
Acetamiprid	0.5	99.2	4.8
Acetamiprid	5	85.1	7.4
Imidacloprid	0.5	99.5	3.9
Imidacloprid	5	89.1	4.5
Thiamethoxam	0.5	89.9	6.5
Thiamethoxam	5	86.8	7.4
Imidaclothiz	0.5	96.7	4.4
Imidaclothiz	5	96.3	3.8
Thiacloprid	0.5	97.5	4.4
Thiacloprid	5	92.4	3.4
Prometon	0.5	97.3	2.4
Prometon	5	101	7.2
Atrazine	0.5	89.1	9
Atrazine	5	83	7.6
Propazine	0.5	94	6.5
Propazine	5	94.6	6
Terbuthylazine	0.5	88.3	3.6
Terbuthylazine	5	89.6	6.1
Cyprazine	0.5	87.5	12.4
Cyprazine	5	87.8	3.4
Metribuzin	0.5	92.9	4.7
Metribuzin	5	97.3	8.6
Ametryn	0.5	96.2	6.5
Ametryn	5	95.7	8.9
Prometryn	0.5	93.1	4.9
Prometryn	5	93.8	6.3
Cyanazine	0.5	95.3	7.1
Cyanazine	5	101.5	7.7
Procyazine	0.5	94.4	5.6
Procyazine	5	95	5.5
Hexazinone	0.5	100.5	8.4
Hexazinone	5	101.6	7.9

Method	Matrix volume / mL	Adsorbent	Solvent	time / min	LOD / (μg L^-1)	Ref.
SPE-HPLC	500	0.1 g of MWCNTs	4 mL of methanol	> 70	thiamethoxam 0.0061, imidacloprid 0.0054, acetamiprid 0.0067	²2 Zhou, Q. X.; Ding, Y. J.; Xiao, J. P.; Anal. Bioanal. Chem. 2006, 385, 1520.
SPE-HPLC	100	(500 mg x 2.8 mL) C₁₈ column	7 mL of methanol	> 20	imidacloprid 0.5	⁴⁰40 Baskaran, S.; Kookana, R. S.; Naidu, R.; J. Chromatogr. A 1997, 787, 271.
SPE-LC-ES/MS	≥1000	0.5 g of graphitized carbon black	6 mL of methylenechloride/methanol (80:20, v/v)2 mL of methanol	> 20	atrazine 0.04 ng^a a Quantitative ion.	⁴¹41 DiCorcia, A.; Crescenzi, C.; Guerriero, E.; Samperi, R.; Environ. Sci. Technol. 1997, 31, 1658.
SPE-HPLC	500	0.1 g of MWCNTs	4 mL of acetonitrile	> 70	atrazine, 0.033; simazine, 0.009	⁴²42 Zhou, Q. X.; Xiao, J. P.; Wang, W. D.; Liu, G. G.; Shi, Q. Z.; Wang, J. H.; Talanta 2006, 68, 1309.
SPE-HPLC	250	0.1 g of MWCNTs	10 mL of methanol,20 mL of	> 50	cyanazine 0.015	⁴³43 Zhou, Q. X.; Ding, Y. J.; Xia, J. P.; Chromatographia 2007, 65, 25.
SPE-HPLC	500	0.1 g of MWCNTs	methanol, 6mL of dichloromethane	> 70	prometryn 0.0008	⁴⁴44 Zhou, Q. X.; Xiao, J. P.; Ding, Y. J.; Anal. Chim. Acta 2007, 602, 223.
SPE-HPLC	100	0.1 g of MWCNTs	4mL of ethyl acetate, 3 mL of methanol	> 30	atrazine 0.02	⁴⁵45 Min, G.; Wang, S.; Zhu, H. P.; Fang, G. Z.; Zhang, Y.; Sci. Total Environ. 2008, 396, 79.
SPE-HPLC	100	1.0 g of bamboo charcoal	20 mL of acetonitrile	> 50	simazine 0.1; atrazine 0.1	⁴⁶46 Zhao, R. S.; Yuan, J. P.; Jiang, T.; Shi, J. B.; Cheng, C. G.; Talanta 2008, 76, 956.
This work	40	≤ 6 mL of graphene (3 mg mL^-1)	8 mL of acetonitrile	< 20	acetaniprid, 0.10; imidacloprid, 0.05; thiamethoxam, 0.15; imidaclothiz, 0.05; thiacloprid, 0.03; prometon, 0.09; atrazine, 0.12; propazine, 0.15; terbuthylazine, 0.04; cyprazine, 0.25; metribuzin, 0.23; ametryn, 0.12;prometryn, 0.09; cyanazine, 0.36;procyazine, 0.40; hexazinone, 0.26	This work

Analyte	Tap water			River water
Analyte	Recovery / %	RSD / %	Found / (μg L^-1)	Recovery / %	RSD / %	Xiaojia River / (μg L^-1)	Jimgmi River / (μg L^-1)
Acetamiprid	96.0	7.8	nd	94.3	7.0	nd	0.2
Imidacloprid	100.3	13.0	nd	91.5	3.7	nd	nd
Thiamethoxam	92.7	5.6	nd	97.9	4.1	nd	nd
Imidaclothiz	102.2	2.9	nd	92.5	2.3	nd	nd
Thiacloprid	98.1	6.3	nd	91.1	9	nd	nd
Prometon	100.2	3.3	nd	101.7	5.4	nd	nd
Atrazine	94.1	3.8	nd	97.8	5.7	100	nd
Propazine	102.2	3.0	nd	101.0	4.3	nd	nd
Terbuthylazine	98.5	2.9	nd	96.0	4.1	nd	nd
Cyprazine	97.6	6.3	nd	96.5	4.7	nd	nd
Metribuzin	97.5	9.7	nd	96.1	6.5	nd	nd
Ametryn	96.0	2.5	nd	98.8	5.0	nd	nd
Prometryn	99.1	5.5	nd	98.9	6.9	nd	nd
Cyanazine	95.5	7.8	nd	95.2	4.8	nd	nd
Procyazine	91.6	4.5	nd	93.8	8.5	nd	nd
Hexazinone	93.7	3.9	nd	94.0	4.1	nd	nd

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