Solid phase extraction and high performance liquid chromatography with tetraaza[2]arene[2]triazine-bonded silica gel adsorbent for determination of nitrophenols and diethylstilbestrol in river water

doi:10.3724/SP.J.1123.2019.06022

Abstract

Abstract:

A novel method based on solid phase extraction (SPE)-high performance liquid chromatography (HPLC) was developed for the simultaneous determination of nitrophenols and diethylstilbestrol in river water. Tetraaza[2]arene[2]triazine-bonded silica gel, a homemade SPE adsorbent, was used to enrich the nitrophenols and diethylstilbestrol, and the optimal SPE and HPLC conditions were established. The sample solution was adjusted to pH 5, purified with a lab-made solid phase extraction column, and then eluted with 2 mL ammonia-methanol (2:98, v/v). The enriched sample was separated on a C8 column with methanol and 0.1% phosphoric acid solution as mobile phases in a gradient elution. Under the optimized conditions, the limits of detection (LOD, S/N=3) for the four target analytes were 0.03-0.3 μg/L, and the limits of quantification (LOQ, S/N=10) were 0.1-1.0 μg/L. The recoveries were 75.5%-104.2%, and the relative standard deviations (RSD, n=5) were less than 6.3%. The proposed method is accurate and reliable, and it has been successfully used for determining nitrophenols and diethylstilbestrol in river water.

Key words: tetraaza[2]arene[2]triazine, solid phase extraction(SPE), high performance liquid chromatography (HPLC), nitrophenol, diethylstilbestrol, river water

PENG Zifang, LI Qin, ZHANG Guangrui, ZHAO Wuduo, LIAN Hongzhen, ZHANG Shusheng. Solid phase extraction and high performance liquid chromatography with tetraaza[2]arene[2]triazine-bonded silica gel adsorbent for determination of nitrophenols and diethylstilbestrol in river water[J]. Chinese Journal of Chromatography, 2020, 38(1): 143-148.

Figures/Tables 5

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Analyte	Regression equation	R²	LOD/ (μg/L)	LOQ/ (μg/L)
y: peak area; x: mass concentration, μ g/L.
p-Nitrophenol	y=55.995x-0.5002	0.9993	0.300	1.00
2, 4-Dinitrophenol	y=369.96x+1.4519	0.9995	0.100	0.300
2, 4, 6-Trinitrophenol	y=22.786x+4.1287	0.9999	0.030	0.100
Diethylstilbestrol	y=51.349x+0.2886	0.9998	0.030	0.100

Analyte	Regression equation	R²	LOD/ (μg/L)	LOQ/ (μg/L)
y: peak area; x: mass concentration, μ g/L.
p-Nitrophenol	y=55.995x-0.5002	0.9993	0.300	1.00
2, 4-Dinitrophenol	y=369.96x+1.4519	0.9995	0.100	0.300
2, 4, 6-Trinitrophenol	y=22.786x+4.1287	0.9999	0.030	0.100
Diethylstilbestrol	y=51.349x+0.2886	0.9998	0.030	0.100

Sample	Analyte	Background/ (μg/L)	Spiked level/ (μg/L)	Found/ (μg/L)	Recovery/ %	RSD/ %
-: not detected
Yellow River water	p-nitrophenol	1.50	1.00	2.28	78.0	5.60
			2.00	3.01	75.5	5.40
			10.00	9.07	75.7	6.30
	2, 4-dinitrophenol	-	2.00	1.69	84.5	3.61
			5.00	4.25	85.0	2.20
			10.00	8.84	88.4	4.83
	2, 4, 6-trinitrophenol	1.40	1.00	2.28	88.0	2.43
			2.00	3.08	84.3	1.90
			10.00	9.36	79.6	3.42
	diethylstilbestrol	0.24	0.50	0.68	88.0	3.40
			2.00	2.32	104.2	5.20
			10.0	9.59	93.4	4.11
Jinshui River water	p-nitrophenol	1.20	1.00	2.01	81.2	3.11
			2.00	2.56	80.1	5.10
			5.00	4.80	77.4	2.00
	2, 4-dinitrophenol	2.30	2.00	2.95	86.2	3.67
			4.00	5.65	83.8	3.40
			10.00	10.75	84.5	5.52
	2, 4, 6-trinitrophenol	2.60	2.00	4.31	85.5	2.43
			4.00	5.84	81.0	2.80
			10.00	11.80	92.0	4.30
	diethylstilbestrol	1.60	0.50	2.04	87.7	4.22
			2.00	3.42	91.1	3.08
			10.00	10.58	89.8	2.82

Sample	Analyte	Background/ (μg/L)	Spiked level/ (μg/L)	Found/ (μg/L)	Recovery/ %	RSD/ %
-: not detected
Yellow River water	p-nitrophenol	1.50	1.00	2.28	78.0	5.60
			2.00	3.01	75.5	5.40
			10.00	9.07	75.7	6.30
	2, 4-dinitrophenol	-	2.00	1.69	84.5	3.61
			5.00	4.25	85.0	2.20
			10.00	8.84	88.4	4.83
	2, 4, 6-trinitrophenol	1.40	1.00	2.28	88.0	2.43
			2.00	3.08	84.3	1.90
			10.00	9.36	79.6	3.42
	diethylstilbestrol	0.24	0.50	0.68	88.0	3.40
			2.00	2.32	104.2	5.20
			10.0	9.59	93.4	4.11
Jinshui River water	p-nitrophenol	1.20	1.00	2.01	81.2	3.11
			2.00	2.56	80.1	5.10
			5.00	4.80	77.4	2.00
	2, 4-dinitrophenol	2.30	2.00	2.95	86.2	3.67
			4.00	5.65	83.8	3.40
			10.00	10.75	84.5	5.52
	2, 4, 6-trinitrophenol	2.60	2.00	4.31	85.5	2.43
			4.00	5.84	81.0	2.80
			10.00	11.80	92.0	4.30
	diethylstilbestrol	1.60	0.50	2.04	87.7	4.22
			2.00	3.42	91.1	3.08
			10.00	10.58	89.8	2.82

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