Test of Various Plasticizers in Groundwater by Using SPME-GC-MS

doi:10.12141/j.issn.1000-565X.210494

Abstract

Abstract:

The pollution problem of plasticizers in water has attracted more and more attention, and the research on their testing methods is also increasing, but the research on testing different types of plasticizers at the same time is relatively rare. And most of these studies use headspace solid phase microextraction, which is difficult to ensure good extraction efficiency and low detection limit. Therefore, this paper developed a SPME-GC-MS method to test 11 plasticizers included in two types in groundwater by using immersion solid phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS). This method used 65 μm DVB/PDMS fiber, and the extraction was carried out at 80 ℃ for 50 min with a constant stirring speed of 1 000 r/min. The fiber was introduced into GC injector port, the extract was desorbed at 270 ℃ for 2.5 min and then detected by GC-MS. Qualitative analysis was performed by using retention time and characteristic ion, and quantitative by internal standard method. The results show that the linearity of 11 plasticizers is good in the range of 0.1 ~ 2.0 μg/L and the correlation coefficients are greater than 0.996; the detection limit is 0.03 ~ 0.06 μg/L; the recovery is 60.9% ~ 128.0%; and the relative standard deviation (RSD) is 6.68% ~ 19.00%. The proposed method is simple, reliable and sensitive, and it’s suitable for the determination of phthalate esters and adipate esters in groundwater. Moreover, aiming at the blank interference in plasticizer analysis, this paper conducted an in-depth study on this difficulty for the first time, carried out a detailed analysis from various aspects such as reagents, consumables and instrument maintenance, and proposed practical and operable solutions, which can effectively reduce the blank interference of plasticizers in the analysis process and further ensure the reliability of the analysis results.

Key words: groundwater, plasticizer, phthalate esters, adipate esters, solid phase microextraction, gas chromatography-mass spectrometry

CLC Number:

X832

XU Ruijie, CHEN Kefu, ZHAO Weihong, et al. Test of Various Plasticizers in Groundwater by Using SPME-GC-MS[J]. Journal of South China University of Technology(Natural Science Edition), 2022, 50(8): 109-118.

Figures/Tables 13

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化合物	化合物简称	CAS号	定量离子质荷比	定性离子质荷比
邻苯二甲酸二甲酯	DMP	131-11-3	163	77、194
邻苯二甲酸二乙酯	DEP	84-66-2	149	177、222
邻苯二甲酸二丁酯	DBP	84-74-2	149	150、76
邻苯二甲酸二丁基苄基酯	BBP	85-68-7	149	91、206
邻苯二甲酸二（2-乙基己基）酯	DEHP	117-81-7	149	167、279
邻苯二甲酸二正辛酯	DNOP	117-84-0	149	279、150
邻苯二甲酸二烯丙酯	DAP	131-17-9	149	41、189
己二酸二乙酯	DEA	141-28-6	111	157、128
己二酸二丁酯	DBA	105-99-7	129	185、111
己二酸二异丁酯	DIBA	141-04-8	129	185、111
己二酸二（2-乙基己基）酯	DEHA	103-23-1	129	112、147
邻苯二甲酸二己酯（内标）	DNHP	84-75-3	149	43

待测物	回归方程	相关系数	检出限/（μg·L^-1）
DEA	y = 0.281 6x - 0.001 7	0.999	0.04
DMP	y = 0.280 1x + 0.004 4	0.998	0.03
DEP	y = 1.019x - 0.005 7	0.999	0.03
DBA	y = 1.089x - 0.045 4	0.999	0.03
DAP	y = 0.569 7x - 0.028 6	0.999	0.03
DIBA	y = 0.741 7x - 0.028 9	0.999	0.03
DBP	y = 2.964x + 0.059 6	0.997	0.06
BBP	y = 1.178x - 0. 023 6	0.999	0.03
DEHA	y = 0.200 5x - 0.004 2	0.999	0.04
DEHP	y = 0.167 4x + 0.020 6	0.998	0.05
DNOP	y = 0.109 3x - 0.002 6	0.996	0.05

被测物	加标量/（μg·L^-1）	回收率/%	相对标准偏差/%
DEA	0.1	81.8 ~ 110	13.4
	0.5	79.1 ~ 111	11.7
	1.0	80.7 ~ 108	9.58
DMP	0.1	82.2 ~ 108	11.1
	0.5	99.7 ~ 126	9.83
	1.0	88.2 ~ 120	10.9
DEP	0.1	78.4 ~ 107	13.3
	0.5	91.1 ~ 120	11.9
	1.0	87.6 ~ 109	8.88
DBA	0.1	103 ~ 126	8.47
	0.5	68.7 ~ 99.7	13.2
	1.0	77.2 ~ 98.4	10.6
DAP	0.1	88.4 ~ 117	11.7
	0.5	68.7 ~ 105	16.2
	1.0	83.9 ~ 99.2	6.68
DIBA	0.1	108 ~ 128	6.78
	0.5	66.2 ~ 97.1	13.7
	1.0	78.2 ~ 98.7	10.6
DBP	0.1	62.2 ~ 118	16.4
	0.5	71.4 ~ 94.5	11.2
	1.0	83.0 ~ 114	13.7
BBP	0.1	84.8 ~ 116	11.2
	0.5	62.3 ~ 101	17.6
	1.0	78.9 ~ 99.8	8.67
DEHA	0.1	68.6 ~ 96.5	15.7
	0.5	60.9 ~ 104	19.0
	1.0	77.6 ~ 121	15.7
DEHP	0.1	63.6 ~ 108	15.8
	0.5	73.2 ~ 97.9	12.8
	1.0	84.7 ~ 122	14.0
DNOP	0.1	90.5 ~ 124	10.8
	0.5	65.7 ~ 98.0	13.3
	1.0	93.6 ~ 119	8.63

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