Determination of 20 Pesticide Residues in Red Beet by Modified QuEChERS Method Combined with Gas Chromatography

doi:10.11924/j.issn.1000-6850.casb2021-0684

Abstract

Abstract:

A method was developed to determine 20 pesticide residues in red beet by modified QuEChERS method combined with gas chromatography-electron capture detector. The pesticide residues in the samples were extracted by acetonitrile and cleaned up by dispersive solid-phase extraction using MWCNTs, after filtration, they were separated on RTX-1 chromatographic column, determined by gas chromatography, and quantified by the external standard method. The temperature-programmed conditions of gas chromatography were tested, and the effects of different extraction solvents and purification methods on the detection results were investigated. The results showed that under the optimized conditions, good linear relations were obtained in the range of 0.01-0.50 mg/L (Atrazine was in the range of 0.03-0.50 mg/L), the correlation coefficients (R²) were all higher than 0.99, and 20 pesticides were well separated. The pre-treatment condition was as follow: acetonitrile: sample was 2:1, and the amount of MWCNTs was 10 mg. The average recoveries of red beet were 62.0%-116.5% at three spiked concentration levels with relative standard deviations (RSDs) of 1.9%-10.9%, the limits of detection were 0.12 μg/L - 0.063 mg/L, and the limits of quantitation were 0.4 μg/L - 0.21 mg/L. This method is simple, rapid, accurate, and could be used for the determination of organochlorine and pyrethroid residues in red beet.

Key words: QuEChERS, gas chromatography, multi-walled carbon nanotubes, red beet, pesticide residue

CLC Number:

Liu Lin, Ma Tengfei, Jia Sunyue, Zhou Qin, Wang Xiwei. Determination of 20 Pesticide Residues in Red Beet by Modified QuEChERS Method Combined with Gas Chromatography[J]. Chinese Agricultural Science Bulletin, 2021, 37(35): 110-117.

Figures/Tables 7

References 36

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序号	农药名称	保留时间/ min	线性回归方程	相关系数 (R²)	线性范围/ (mg/L)	检出限(LOD)/ (mg/L)	定量限(LOQ)/ (mg/L)
1	α-六六六	5.950	Y=5403880X+843.20	0.9994	0.01-0.50	0.0068	0.023
2	β-六六六	6.301	Y=2351319X+13673.71	0.9991	0.01-0.50	0.0254	0.085
3	莠去津	6.516	Y=77612.16X+4602.97	0.9974	0.03-0.50	0.0630	0.210
4	γ-六六六	6.745	Y=4267368X+2130.29	0.9994	0.01-0.50	0.0201	0.067
5	δ-六六六	6.899	Y=4335205X-19409.3	0.9995	0.01-0.50	0.0187	0.062
6	百菌清	7.311	Y=3352703X+16.89	0.9993	0.01-0.50	0.0219	0.073
7	七氯	9.200	Y=3122723X+20282.27	0.9991	0.01-0.50	0.0250	0.083
8	艾氏剂	10.301	Y=4244097X+1214.20	0.9994	0.01-0.50	0.0198	0.066
9	pp'-滴滴伊	13.329	Y=4572184X-5123.11	0.9995	0.01-0.50	0.0190	0.063
10	异狄氏剂	13.870	Y=3526679X+143758.6	0.9950	0.01-0.50	0.0001	0.000
11	pp'-滴滴滴	14.451	Y=2084406X+34237.52	0.9969	0.01-0.50	0.0047	0.016
12	op'-滴滴涕	14.716	Y=5183422X+29151.38	0.9995	0.01-0.50	0.0006	0.002
13	pp'-滴滴涕	15.733	Y=3169636X+223.16	0.9995	0.01-0.50	0.0189	0.063
14	甲氰菊酯	17.659	Y=1003682X+26046.62	0.9951	0.01-0.50	0.0100	0.033
15	氯氟氰菊酯	19.232	Y=3424542X-73067.19	0.9964	0.01-0.50	0.0087	0.029
16	顺式二氯苯醚菊酯	20.492	Y=690182.7X+6660.86	0.9996	0.01-0.50	0.0025	0.008
17	二氯苯醚菊酯	20.750	Y=622104.3X+5767.925	0.9995	0.01-0.50	0.0039	0.013
18	氟氯氰菊酯	22.015	Y=617136.6X-327.47	0.9998	0.01-0.50	0.0122	0.041
19	氰戊菊酯	25.140	Y=1669978X-7717.494	0.9999	0.01-0.50	0.0019	0.006
20	溴氰菊酯	27.998	Y=1766025X+24795.23	0.9959	0.01-0.50	0.0167	0.056

序号	农药名称	保留时间/ min	线性回归方程	相关系数 (R²)	线性范围/ (mg/L)	检出限(LOD)/ (mg/L)	定量限(LOQ)/ (mg/L)
1	α-六六六	5.950	Y=5403880X+843.20	0.9994	0.01-0.50	0.0068	0.023
2	β-六六六	6.301	Y=2351319X+13673.71	0.9991	0.01-0.50	0.0254	0.085
3	莠去津	6.516	Y=77612.16X+4602.97	0.9974	0.03-0.50	0.0630	0.210
4	γ-六六六	6.745	Y=4267368X+2130.29	0.9994	0.01-0.50	0.0201	0.067
5	δ-六六六	6.899	Y=4335205X-19409.3	0.9995	0.01-0.50	0.0187	0.062
6	百菌清	7.311	Y=3352703X+16.89	0.9993	0.01-0.50	0.0219	0.073
7	七氯	9.200	Y=3122723X+20282.27	0.9991	0.01-0.50	0.0250	0.083
8	艾氏剂	10.301	Y=4244097X+1214.20	0.9994	0.01-0.50	0.0198	0.066
9	pp'-滴滴伊	13.329	Y=4572184X-5123.11	0.9995	0.01-0.50	0.0190	0.063
10	异狄氏剂	13.870	Y=3526679X+143758.6	0.9950	0.01-0.50	0.0001	0.000
11	pp'-滴滴滴	14.451	Y=2084406X+34237.52	0.9969	0.01-0.50	0.0047	0.016
12	op'-滴滴涕	14.716	Y=5183422X+29151.38	0.9995	0.01-0.50	0.0006	0.002
13	pp'-滴滴涕	15.733	Y=3169636X+223.16	0.9995	0.01-0.50	0.0189	0.063
14	甲氰菊酯	17.659	Y=1003682X+26046.62	0.9951	0.01-0.50	0.0100	0.033
15	氯氟氰菊酯	19.232	Y=3424542X-73067.19	0.9964	0.01-0.50	0.0087	0.029
16	顺式二氯苯醚菊酯	20.492	Y=690182.7X+6660.86	0.9996	0.01-0.50	0.0025	0.008
17	二氯苯醚菊酯	20.750	Y=622104.3X+5767.925	0.9995	0.01-0.50	0.0039	0.013
18	氟氯氰菊酯	22.015	Y=617136.6X-327.47	0.9998	0.01-0.50	0.0122	0.041
19	氰戊菊酯	25.140	Y=1669978X-7717.494	0.9999	0.01-0.50	0.0019	0.006
20	溴氰菊酯	27.998	Y=1766025X+24795.23	0.9959	0.01-0.50	0.0167	0.056

序号	农药名称	加标浓度/ (mg/kg)	平均回收率/%	RSD/%	序号	农药名称	加标浓度/ (mg/kg)	平均回收率/%	RSD/%
1	α-六六六	0.04	62.5	4.6	11	pp'-滴滴滴	0.05	114.1	3.6
		0.08	62.8	2.7			0.1	116.2	3.5
		0.16	70.0	6.4			0.2	113.8	3.4
2	β-六六六	0.05	80.0	8.8	12	op'-滴滴涕	0.05	116.2	2.8
		0.1	107.4	3.3			0.1	114.5	2.3
		0.2	111.7	3.4			0.2	110.5	2.5
3	莠去津	0.1	82.8	8.3	13	pp'-滴滴涕	0.05	97.5	9.5
		0.2	86.2	2.5			0.1	108.3	5.9
		0.4	73.4	8.3			0.2	105.8	3.9
4	γ-六六六	0.04	114.9	3.5	14	甲氰菊酯	0.08	116.5	2.8
		0.08	109.2	4.2			0.16	112.0	4.2
		0.16	111.2	3.6			0.32	112.8	6.4
5	δ-六六六	0.05	116.0	2.6	15	氯氟氰菊酯	0.05	62.0	6.4
		0.1	109.5	3.0			0.1	72.3	10.9
		0.2	111.0	2.7			0.2	68.5	8.6
6	百菌清	0.05	81.4	7.1	16	顺式二氯苯醚菊酯	0.08	113.5	3.8
		0.1	114.2	3.9			0.16	111.4	2.4
		0.2	80.6	8.1			0.32	112.0	3.3
7	七氯	0.05	107.4	8.9	17	二氯苯醚菊酯	0.08	106.7	9.3
		0.1	95.3	9.5			0.16	108.9	8.5
		0.2	107.7	6.1			0.32	108.2	4.0
8	艾氏剂	0.05	107.5	9.8	18	氟氯氰菊酯	0.08	87.5	5.0
		0.1	111.2	4.0			0.16	76.5	9.5
		0.2	103.3	8.4			0.32	110.7	7.2
9	pp'-滴滴伊	0.05	113.6	2.0	19	氰戊菊酯	0.08	84.2	8.9
		0.1	112.0	2.6			0.16	84.4	4.8
		0.2	107.8	4.3			0.32	101.2	9.5
10	异狄氏剂	0.05	71.7	9.8	20	溴氰菊酯	0.08	62.2	7.0
		0.1	92.2	10.3			0.16	62.7	2.6
		0.2	110.1	5.9			0.32	62.7	1.9

序号	农药名称	加标浓度/ (mg/kg)	平均回收率/%	RSD/%	序号	农药名称	加标浓度/ (mg/kg)	平均回收率/%	RSD/%
1	α-六六六	0.04	62.5	4.6	11	pp'-滴滴滴	0.05	114.1	3.6
		0.08	62.8	2.7			0.1	116.2	3.5
		0.16	70.0	6.4			0.2	113.8	3.4
2	β-六六六	0.05	80.0	8.8	12	op'-滴滴涕	0.05	116.2	2.8
		0.1	107.4	3.3			0.1	114.5	2.3
		0.2	111.7	3.4			0.2	110.5	2.5
3	莠去津	0.1	82.8	8.3	13	pp'-滴滴涕	0.05	97.5	9.5
		0.2	86.2	2.5			0.1	108.3	5.9
		0.4	73.4	8.3			0.2	105.8	3.9
4	γ-六六六	0.04	114.9	3.5	14	甲氰菊酯	0.08	116.5	2.8
		0.08	109.2	4.2			0.16	112.0	4.2
		0.16	111.2	3.6			0.32	112.8	6.4
5	δ-六六六	0.05	116.0	2.6	15	氯氟氰菊酯	0.05	62.0	6.4
		0.1	109.5	3.0			0.1	72.3	10.9
		0.2	111.0	2.7			0.2	68.5	8.6
6	百菌清	0.05	81.4	7.1	16	顺式二氯苯醚菊酯	0.08	113.5	3.8
		0.1	114.2	3.9			0.16	111.4	2.4
		0.2	80.6	8.1			0.32	112.0	3.3
7	七氯	0.05	107.4	8.9	17	二氯苯醚菊酯	0.08	106.7	9.3
		0.1	95.3	9.5			0.16	108.9	8.5
		0.2	107.7	6.1			0.32	108.2	4.0
8	艾氏剂	0.05	107.5	9.8	18	氟氯氰菊酯	0.08	87.5	5.0
		0.1	111.2	4.0			0.16	76.5	9.5
		0.2	103.3	8.4			0.32	110.7	7.2
9	pp'-滴滴伊	0.05	113.6	2.0	19	氰戊菊酯	0.08	84.2	8.9
		0.1	112.0	2.6			0.16	84.4	4.8
		0.2	107.8	4.3			0.32	101.2	9.5
10	异狄氏剂	0.05	71.7	9.8	20	溴氰菊酯	0.08	62.2	7.0
		0.1	92.2	10.3			0.16	62.7	2.6
		0.2	110.1	5.9			0.32	62.7	1.9