Determination of 12 triazine herbicides in drinking water by SPE-UPLC-MS/MS

Abstract

Abstract:

Objective To establish a ultra-high performance liquid chromatography-tandem mass spectrometry（SPE-UPLC-MS/MS） method for the determination of 12 triazine herbicides in drinking water. Methods Water samples were spiked with internal standards and extracted using Supelclean ENVI-Chrom P SPE cartridges，followed by detection via UPLC-MS/MS. Quantification was performed using the internal standard method. Results The 12 triazine herbicides exhibited good linearity in the range of 0.1 to 50.0 ng/mL（r≥0.999）. With a sample volume of 200 mL，the method detection limits（MDLs） for the 12 triazine herbicides ranged from 0.05 to 0.14 ng/L，and the method quantification limits（MQLs） ranged from 0.15 to 0.42 ng/L. For the three concentration levels（5，50，and 200 ng/L），the spike recovery rates ranged from 83.6% to 101.1% in pure water and from 85.6% to 100.4% in tap water. The relative standard deviations（RSDs） were 1.1%-4.3% and 1.0%-6.0%，respectively. Conclusion The established method is sensitive，reliable，and suitable for the detection of 12 triazine herbicides in drinking water.

Key words: Triazine herbicides, Solid-phase extraction, Supelclean ENVI-Chrom P SPE cartridges, Ultra-high performance liquid chromatography-tandem mass spectrometry, Internal standard method, Drinking water

CLC Number:

R115

ZHANG Jue, DAI Jing, MIN Wei, HAN Zhebin, ZHENG Rong, ZHAO Yijing. Determination of 12 triazine herbicides in drinking water by SPE-UPLC-MS/MS. [J]OCCUPATION AND HEALTH, 2026, 42(17): 2337-2342.

Figures/Tables 4

References 24

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化合物名称	CAS号	母离子（m/z）	子离子（m/z）	锥孔电压（V）	碰撞能量（eV）	保留时间（min）
莠去津	1912-24-9	215.882	173.889^a/95.859	28	14/22	4.78
西玛津	122-34-9	201.862	123.875^a/131.815	26	16/16	4.01
氰草津	21725-46-2	240.892	213.890^a/103.816	22	14/28	4.08
扑灭津	139-40-2	229.848	187.878^a/145.786	4	14/20	5.50
特丁津	5915-41-3	229.848	173.828^a/95.880	2	14/24	5.66
西草净	1014-70-6	213.949	123.871^a/95.885	2	16/22	3.43
莠灭净	834-12-8	227.979	185.873^a/95.880	2	16/24	4.13
扑草净	7287-19-6	241.881	157.824^a/199.915	74	20/16	4.84
环嗪酮	51235-04-2	252.959	170.913^a/100.833	14	12/36	3.77
嗪草酮	21087-64-9	214.875	186.889^a/130.814	36	16/18	4.20
莠去通	1610-17-9	211.973	169.862^a/99.785	2	16/22	2.98
扑灭通	1610-18-0	226.003	183.906^a/141.878	2	16/20	3.54
莠去津-d5	163165-75-1	220.912	178.865^a/100.836	22	16/22	4.75
西玛津-d10	220621-39-6	211.882	136.893^a/133.960	26	18/16	3.95
氰草津-d5	1190003-29-2	245.986	218.919^a/100.891	26	14/24	4.07
扑灭津-d14	1219802-87-5	243.938	195.931^a/147.859	68	16/22	5.42
特丁津-d5	222986-60-9	234.878	178.916^a/136.882	54	14/22	5.63
扑草净-d14	1202864-57-0	256.089	159.826^a/207.960	2	24/18	4.72
环嗪酮-d6	1219804-22-4	258.999	176.896^a/90.938	20	14/28	3.75
扑灭通-d14	1219803-45-8	239.965	192.022^a/143.886	76	18/22	3.47

化合物名称	CAS号	母离子（m/z）	子离子（m/z）	锥孔电压（V）	碰撞能量（eV）	保留时间（min）
莠去津	1912-24-9	215.882	173.889^a/95.859	28	14/22	4.78
西玛津	122-34-9	201.862	123.875^a/131.815	26	16/16	4.01
氰草津	21725-46-2	240.892	213.890^a/103.816	22	14/28	4.08
扑灭津	139-40-2	229.848	187.878^a/145.786	4	14/20	5.50
特丁津	5915-41-3	229.848	173.828^a/95.880	2	14/24	5.66
西草净	1014-70-6	213.949	123.871^a/95.885	2	16/22	3.43
莠灭净	834-12-8	227.979	185.873^a/95.880	2	16/24	4.13
扑草净	7287-19-6	241.881	157.824^a/199.915	74	20/16	4.84
环嗪酮	51235-04-2	252.959	170.913^a/100.833	14	12/36	3.77
嗪草酮	21087-64-9	214.875	186.889^a/130.814	36	16/18	4.20
莠去通	1610-17-9	211.973	169.862^a/99.785	2	16/22	2.98
扑灭通	1610-18-0	226.003	183.906^a/141.878	2	16/20	3.54
莠去津-d5	163165-75-1	220.912	178.865^a/100.836	22	16/22	4.75
西玛津-d10	220621-39-6	211.882	136.893^a/133.960	26	18/16	3.95
氰草津-d5	1190003-29-2	245.986	218.919^a/100.891	26	14/24	4.07
扑灭津-d14	1219802-87-5	243.938	195.931^a/147.859	68	16/22	5.42
特丁津-d5	222986-60-9	234.878	178.916^a/136.882	54	14/22	5.63
扑草净-d14	1202864-57-0	256.089	159.826^a/207.960	2	24/18	4.72
环嗪酮-d6	1219804-22-4	258.999	176.896^a/90.938	20	14/28	3.75
扑灭通-d14	1219803-45-8	239.965	192.022^a/143.886	76	18/22	3.47

化合物	线性方程	线性范围（ng/mL）	r值	200 mL空白样品加标0.1 ng后测定值（ng/L，n=6）	方法检出限（ng/L）	方法定量限（ng/L）
莠去津	Y=0.109 5X+0.002 8	0.1~50.0	0.999 7	0.48/0.51/0.51/0.46/0.50/0.48	0.11	0.33
西玛津	Y=0.091 1X+0.002 7	0.1~50.0	0.999 7	0.48/0.47/0.46/0.49/0.48/0.48	0.07	0.21
氰草津	Y=0.087 7X+0.001 1	0.1~50.0	0.999 6	0.49/0.46/0.49/0.48/0.48/0.47	0.08	0.24
扑灭津	Y=0.174 2X+0.004 1	0.1~50.0	0.999 6	0.47/0.42/0.43/0.42/0.41/0.43	0.11	0.33
特丁津	Y=0.175 2X+0.004 7	0.1~50.0	0.999 8	0.48/0.51/0.49/0.48/0.50/0.46	0.10	0.30
西草净	Y=0.382 9X+0.007 0	0.1~50.0	0.999 9	0.49/0.50/0.52/0.50/0.50/0.50	0.05	0.15
莠灭净	Y=0.885 6X+0.014 0	0.1~50.0	0.999 0	0.48/0.49/0.47/0.49/0.48/0.48	0.05	0.15
扑草净	Y=0.047 1X+0.001 1	0.1~50.0	0.999 7	0.41/0.44/0.42/0.46/0.42/0.43	0.10	0.30
环嗪酮	Y=0.098 7X+0.002 3	0.1~50.0	0.999 4	0.44/0.41/0.45/0.44/0.45/0.43	0.10	0.30
嗪草酮	Y=0.130 5X+0.001 5	0.1~50.0	0.999 5	0.46/0.49/0.43/0.44/0.48/0.48	0.13	0.39
莠去通	Y=0.611 2X+0.016 1	0.1~50.0	0.999 1	0.46/0.45/0.51/0.44/0.46/0.48	0.14	0.42
扑灭通	Y=0.461 2X+0.011 3	0.1~50.0	0.999 4	0.49/0.48/0.50/0.51/0.47/0.49	0.08	0.24

化合物	线性方程	线性范围（ng/mL）	r值	200 mL空白样品加标0.1 ng后测定值（ng/L，n=6）	方法检出限（ng/L）	方法定量限（ng/L）
莠去津	Y=0.109 5X+0.002 8	0.1~50.0	0.999 7	0.48/0.51/0.51/0.46/0.50/0.48	0.11	0.33
西玛津	Y=0.091 1X+0.002 7	0.1~50.0	0.999 7	0.48/0.47/0.46/0.49/0.48/0.48	0.07	0.21
氰草津	Y=0.087 7X+0.001 1	0.1~50.0	0.999 6	0.49/0.46/0.49/0.48/0.48/0.47	0.08	0.24
扑灭津	Y=0.174 2X+0.004 1	0.1~50.0	0.999 6	0.47/0.42/0.43/0.42/0.41/0.43	0.11	0.33
特丁津	Y=0.175 2X+0.004 7	0.1~50.0	0.999 8	0.48/0.51/0.49/0.48/0.50/0.46	0.10	0.30
西草净	Y=0.382 9X+0.007 0	0.1~50.0	0.999 9	0.49/0.50/0.52/0.50/0.50/0.50	0.05	0.15
莠灭净	Y=0.885 6X+0.014 0	0.1~50.0	0.999 0	0.48/0.49/0.47/0.49/0.48/0.48	0.05	0.15
扑草净	Y=0.047 1X+0.001 1	0.1~50.0	0.999 7	0.41/0.44/0.42/0.46/0.42/0.43	0.10	0.30
环嗪酮	Y=0.098 7X+0.002 3	0.1~50.0	0.999 4	0.44/0.41/0.45/0.44/0.45/0.43	0.10	0.30
嗪草酮	Y=0.130 5X+0.001 5	0.1~50.0	0.999 5	0.46/0.49/0.43/0.44/0.48/0.48	0.13	0.39
莠去通	Y=0.611 2X+0.016 1	0.1~50.0	0.999 1	0.46/0.45/0.51/0.44/0.46/0.48	0.14	0.42
扑灭通	Y=0.461 2X+0.011 3	0.1~50.0	0.999 4	0.49/0.48/0.50/0.51/0.47/0.49	0.08	0.24

化合物	加标浓度（ng/L）	纯水（n=6）			自来水（n=6）
化合物	加标浓度（ng/L）	实测浓度（ng/L）	RSD （%）	回收率（%）	实测浓度（ng/L）	RSD（%）	回收率（%）
莠去津	5	4.94	4.3	98.8	4.87	2.8	97.4
	50	47.39	1.5	94.8	48.38	4.2	96.8
	200	190.94	1.8	95.5	198.17	1.0	99.1
西玛津	5	5.03	2.6	100.6	4.94	1.7	98.8
	50	47.51	2.4	95.0	49.21	2.5	98.4
	200	191.52	3.2	95.8	197.77	2.3	98.9
氰草津	5	4.98	2.2	99.6	4.79	3.6	95.8
	50	46.93	3.0	93.9	47.00	2.9	94.0
	200	187.11	1.4	93.6	193.73	1.8	96.9
扑灭津	5	4.91	3.5	98.2	5.00	2.3	100.1
	50	48.02	2.5	96.0	49.46	3.7	98.9
	200	192.72	2.8	96.4	200.77	1.8	100.4
特丁津	5	5.03	2.7	100.6	4.95	5.2	99.0
	50	48.05	2.0	96.1	49.14	1.3	98.3
	200	193.69	1.2	96.8	198.04	1.3	99.0
西草净	5	4.71	2.7	94.2	4.52	5.6	90.3
	50	47.05	1.8	94.1	44.13	3.5	88.3
	200	188.41	2.3	94.2	183.15	3.6	91.6
莠灭净	5	4.89	3.9	97.8	4.45	6.0	89.0
	50	48.33	1.6	96.7	42.82	3.3	85.6
	200	196.72	1.1	98.4	181.33	4.0	90.7
扑草净	5	4.53	2.2	90.5	4.30	3.1	86.0
	50	41.80	2.0	83.6	43.69	4.6	87.4
	200	182.85	4.2	91.4	181.77	3.0	90.9
环嗪酮	5	4.98	1.8	99.6	4.85	2.6	97.0
	50	48.87	1.7	97.7	47.82	1.6	95.6
	200	190.12	1.5	95.1	193.98	2.0	97.0
嗪草酮	5	5.05	2.1	101.1	4.77	3.1	95.3
	50	48.00	2.3	96.0	47.08	3.4	94.2
	200	194.01	2.1	97.0	191.75	2.0	95.9
莠去通	5	4.99	2.0	99.9	4.81	2.1	96.2
	50	48.34	1.4	96.7	48.67	1.1	97.3
	200	190.26	2.7	95.1	195.34	2.6	97.7
扑灭通	5	4.82	1.7	96.4	4.80	2.7	96.0
	50	46.63	2.1	93.3	48.51	2.3	97.0
	200	184.97	1.8	92.5	197.37	1.0	98.7