水样生物毒性评估的样品前处理方法研究进展

doi:10.11894/iwt.2021-0181

摘要/Abstract

摘要：

生物毒性测试对于水质安全评估至关重要。环境水体含有组成复杂的已知和未知化学物质，而往往这些物质的生物毒性效应只有在高倍浓缩条件下才能产生。为了准确评估水样的生物毒性，需要选择合适的样品前处理方法。对液-液萃取和固相萃取的方法原理以及其在环境水样毒性测试中的应用进行了归纳总结，在此基础上对比分析了二者的适用场景，旨在为水样生物毒性测试选择合适的样品前处理方法提供参考。

关键词: 生物毒性, 前处理方法, 液-液萃取, 固相萃取

Abstract:

Biological toxicity testing is essential for water quality and safety assessment. Environmental water samples represent complex mixtures of known and unknown chemicals, and these chemicals often can induce a variety of biological toxicity effects only underhigh concentration. In order to accurately evaluate the biological toxicity of water and wastewater, appropriate sample extraction methods are of great importance. The principles of liquid-liquid extraction and solid phase extraction were reviewed and their applications in toxicity testing of water and wastewater were summarized. On this basis, the applicable scenarios of the two methods were compared and analyzed, so as to provide theoretical reference for selecting appropriate sample extraction methods for biological toxicity assessment of water and wastewater.

Key words: biological toxicity, extraction methods, liquid-liquid extraction, solid phase extraction

中图分类号:

X703

周嘉伟,何席伟,张徐祥,任洪强. 水样生物毒性评估的样品前处理方法研究进展[J]. 工业水处理, 2021, 41(6): 25-34.

Jiawei Zhou,Xiwei He,Xuxiang Zhang,Hongqiang Ren. Advance in sample extraction methods for biological toxicity assessment of water samples[J]. Industrial Water Treatment, 2021, 41(6): 25-34.

https://www.iwt.cn/CN/Y2021/V41/I6/25

图/表 2

参考文献 83

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生物毒性	水样	过滤	水量	pH	萃取剂	保存	参考文献
发育毒性	地表水	0.45 μm	1 L	0.5	MtBE	冷冻干燥	〔31〕
急性毒性、慢性毒性	工业废水	/	300 mL	<2	环己烷	/	〔32〕
遗传毒性	市政污水，地表水	0.45 μm，0.22 μm	500 mL，2 000 mL	/	二氯甲烷	DMSO	〔27〕
致突变性	饮用水	/	4 L	1~2	乙醚，二氯甲烷	DMSO	〔33〕
内分泌干扰毒性、细胞毒性	饮用水，地表水，市政污水	0.45 μm	1 L	/	乙酸乙酯，300 mL	DMSO，50 μL	〔24〕
发育毒性	地表水	0.45 μm	1 L	0.5	MtBE，100 mL	/	〔34〕
遗传毒性、细胞毒性	饮用水	/	100 mL	< 2	MtBE	/	〔26〕
遗传毒性	地表水	0.4 μm	50 mL	/	二氯甲烷，20 mL	甲醇，1 mL	〔28〕
遗传毒性	地表水	/	800 mL，1 800 mL	/	二氯甲烷	DMSO，0.5 mL	〔29〕
遗传毒性	地表水	0.45 μm	1 L	/	正己烷，50 mL；氯仿，50 mL	DMSO，1 mL	〔30〕
内分泌干扰毒性	市政污水	0.45 μm	500 mL	/	戊烷，50 mL；二氯甲烷，50 mL	/	〔25〕
急性毒性	工业废水	0.45 μm	40 mL	2	二氯甲烷，40 mL	/	〔35〕
内分泌干扰毒性	地表水，市政污水	/	2 L	2.5~3	二氯甲烷，400 mL；丙酮，2 mL；己烷，15 mL	丙酮（50 μL）+BPA-d16（10 μL）+MSTFA（90 μL）	〔36〕
急性毒性	市政污水	0.45 μm	/	7，2，11	二氯甲烷	/	〔37〕

生物毒性	水样	过滤	水量	pH	萃取剂	保存	参考文献
发育毒性	地表水	0.45 μm	1 L	0.5	MtBE	冷冻干燥	〔31〕
急性毒性、慢性毒性	工业废水	/	300 mL	<2	环己烷	/	〔32〕
遗传毒性	市政污水，地表水	0.45 μm，0.22 μm	500 mL，2 000 mL	/	二氯甲烷	DMSO	〔27〕
致突变性	饮用水	/	4 L	1~2	乙醚，二氯甲烷	DMSO	〔33〕
内分泌干扰毒性、细胞毒性	饮用水，地表水，市政污水	0.45 μm	1 L	/	乙酸乙酯，300 mL	DMSO，50 μL	〔24〕
发育毒性	地表水	0.45 μm	1 L	0.5	MtBE，100 mL	/	〔34〕
遗传毒性、细胞毒性	饮用水	/	100 mL	< 2	MtBE	/	〔26〕
遗传毒性	地表水	0.4 μm	50 mL	/	二氯甲烷，20 mL	甲醇，1 mL	〔28〕
遗传毒性	地表水	/	800 mL，1 800 mL	/	二氯甲烷	DMSO，0.5 mL	〔29〕
遗传毒性	地表水	0.45 μm	1 L	/	正己烷，50 mL；氯仿，50 mL	DMSO，1 mL	〔30〕
内分泌干扰毒性	市政污水	0.45 μm	500 mL	/	戊烷，50 mL；二氯甲烷，50 mL	/	〔25〕
急性毒性	工业废水	0.45 μm	40 mL	2	二氯甲烷，40 mL	/	〔35〕
内分泌干扰毒性	地表水，市政污水	/	2 L	2.5~3	二氯甲烷，400 mL；丙酮，2 mL；己烷，15 mL	丙酮（50 μL）+BPA-d16（10 μL）+MSTFA（90 μL）	〔36〕
急性毒性	市政污水	0.45 μm	/	7，2，11	二氯甲烷	/	〔37〕

柱子类型	生物毒性	填料	水样	过滤	水量	pH	流速	洗脱溶剂	保存	参考文献
C18柱	内分泌干扰毒性	6 mL，1 g	市政污水	/	5 L	/	/	甲醇+乙酸乙酯（1∶1）	DMSO，0.5 mL	〔47〕
C18柱	内分泌干扰毒性	/	地表污水	/	/	/	/	乙醚；乙醚+己烷（1∶1）；正己烷	甲醇	〔48〕
C18柱	内分泌干扰毒性	500 mg，6 mL	地表水，饮用水	/	2 L	/	/	正己烷，10 mL；正己烷+二氯甲烷（4∶1），10 mL；二氯甲烷+甲醇（1∶1），10 mL	DMSO，0.2 mL	〔49〕
C18膜片	内分泌干扰毒性	47 mm	市政污水	/	50 mL	/	/	甲醇，10 mL	乙酸乙酯，10 mL	〔50〕
C18膜片	内分泌干扰毒性	47 mm	地表水	/	600 mL	/	/	丙酮+甲醇（1∶9），9 mL	干燥保存	〔40〕
C18膜片	内分泌干扰毒性	47 mm	饮用水、地表水	/	600 mL，1.2 L	/	/	丙酮+甲醇（1∶9），9 mL	干燥保存	〔51〕
HLB	内分泌干扰毒性	500 mg，6 mL	地表水	2 μm	1 L	2	10 mL/min	甲醇，10 mL；丙酮+正己烷（1∶1），10 mL	甲醇，1 mL	〔52〕
HLB+Coconut	细胞毒性、遗传毒性、神经毒性、内分泌干扰毒性	/	市政污水	/	/	/	/	甲醇，10 mL	甲醇，1 mL	〔45〕
HLB	内分泌干扰毒性	6 mL	市政污水	0.7 μm	500 mL	/	/	甲醇+二氯甲烷	DMSO，50 μL	〔53〕
HLB	遗传毒性	200 mg，6 mL	地表水，饮用水	/	2 L	/	/	正己烷，6 mL；乙酸乙酯，6 mL；甲醇，6 mL	DMSO，20 μL	〔43〕
HLB	内分泌干扰毒性	500 mg，6 mL	工业废水	/	/	/	6 mL/min	正己烷+二氯甲烷（7∶3），5 mL；MtBE，5 mL；甲醇，5 mL	DMSO，0.2 mL	〔54〕
HLB	遗传毒性	500 mg，6 mL	地上水，地表水	1.2 μm	62 L	3	5~10 mL/min	丙酮，20 mL	DMSO，100 μL	〔55〕
HLB	内分泌干扰毒性		工业废水	0.7 μm	1 L	/	/	正己烷；二氯甲烷；甲醇	DMSO，1 mL	〔56〕
HLB	内分泌干扰毒性、遗传毒性、致癌毒性	12 mg	市政污水	0.45 μm	/	/	10 mL/min	丙酮+二氯甲烷，10 mL	DMSO，1 mL	〔41〕
HLB	内分泌干扰毒性、致癌毒性	200 mg，6 mL	地表水	/	500 mL	/	1 mL/min	二氯甲烷+正己烷（1∶1），10 mL	正己烷，100 μL	〔57〕
HLB	遗传毒性、内分泌干扰毒性、氧化应激毒性	1 g	饮用水	/	5 L	/	/	甲醇，10 mL	甲醇，1 mL	〔58〕
HLB	内分泌干扰毒性、致癌毒性、急性毒性	200 mg	工业废水，市政污水	2 μm	1.2 L	3	5 mL/min	甲醇，6 mL	甲醇，1 mL	〔59〕
StrataX	内分泌干扰毒性	500 mg，6 mL	地表水	0.8 μm	1 L	3	10 mL/min	甲醇，5 mL；甲醇（0.1%氨水），5 mL	5%甲醇，1 mL	〔60〕
StrataX	内分泌干扰毒性	200 mg	饮用水，地表水，市政污水	/	污水：200 mL，地表水：1 000 mL，饮用水：2 000 mL	2	7~10 mL/min	甲醇，3 mL；乙腈，3 mL；丙酮，3 mL	甲醇，1 mL	〔42〕
XAD	遗传毒性	XAD-4，XAD-8	地表水	0.45 μm	15 L	/	/	丙酮，20 mL	DMSO	〔61〕
XAD	细胞毒性、遗传毒性	110 mL XAD-2，XAD-8	市政污水	1.6 μm	13 L	＜2	/	乙酸乙酯，400 mL	DMSO，130 μL	〔44〕
XAD	细胞毒性	55 mL XAD-2	市政污水，工业废水	/	/	1	/	乙酸乙酯	DMSO	〔62〕
XAD	遗传毒性、细胞毒性	30 mL XAD-2，XAD-8	饮用水	0.45 μm	1 L	＜2		乙酸乙酯，200 mL	DMSO，10 μL	〔63〕
XAD	遗传毒性	40 mL XAD-2	地表水，饮用水	1 μm	/	/	40 mL/min	丙酮，40 mL；丙酮+正己烷（1∶3），120 mL；二氯甲烷，80 mL	DMSO	〔64〕
XAD	细胞毒性	55 mL XAD-2，XAD-8	市政污水	1.6 μm，0.45 μm	2 L	/	/	甲醇；乙酸乙酯；甲醇	DMSO	〔65〕
XAD	遗传毒性	13 mL XAD-2，XAD-8	饮用水	/	20 L	/	/	丙酮	/	〔66〕
XAD	细胞毒性、遗传毒性、致突变性、胚胎毒性、内分泌干扰毒性	XAD-4，XAD-7	市政污水，工业废水	0.45 μm	20 L	2	17 mL/min	甲醇，50 mL；丙酮，50 mL	乙醇+DMSO（1∶2），2 mL	〔46〕

柱子类型	生物毒性	填料	水样	过滤	水量	pH	流速	洗脱溶剂	保存	参考文献
C18柱	内分泌干扰毒性	6 mL，1 g	市政污水	/	5 L	/	/	甲醇+乙酸乙酯（1∶1）	DMSO，0.5 mL	〔47〕
C18柱	内分泌干扰毒性	/	地表污水	/	/	/	/	乙醚；乙醚+己烷（1∶1）；正己烷	甲醇	〔48〕
C18柱	内分泌干扰毒性	500 mg，6 mL	地表水，饮用水	/	2 L	/	/	正己烷，10 mL；正己烷+二氯甲烷（4∶1），10 mL；二氯甲烷+甲醇（1∶1），10 mL	DMSO，0.2 mL	〔49〕
C18膜片	内分泌干扰毒性	47 mm	市政污水	/	50 mL	/	/	甲醇，10 mL	乙酸乙酯，10 mL	〔50〕
C18膜片	内分泌干扰毒性	47 mm	地表水	/	600 mL	/	/	丙酮+甲醇（1∶9），9 mL	干燥保存	〔40〕
C18膜片	内分泌干扰毒性	47 mm	饮用水、地表水	/	600 mL，1.2 L	/	/	丙酮+甲醇（1∶9），9 mL	干燥保存	〔51〕
HLB	内分泌干扰毒性	500 mg，6 mL	地表水	2 μm	1 L	2	10 mL/min	甲醇，10 mL；丙酮+正己烷（1∶1），10 mL	甲醇，1 mL	〔52〕
HLB+Coconut	细胞毒性、遗传毒性、神经毒性、内分泌干扰毒性	/	市政污水	/	/	/	/	甲醇，10 mL	甲醇，1 mL	〔45〕
HLB	内分泌干扰毒性	6 mL	市政污水	0.7 μm	500 mL	/	/	甲醇+二氯甲烷	DMSO，50 μL	〔53〕
HLB	遗传毒性	200 mg，6 mL	地表水，饮用水	/	2 L	/	/	正己烷，6 mL；乙酸乙酯，6 mL；甲醇，6 mL	DMSO，20 μL	〔43〕
HLB	内分泌干扰毒性	500 mg，6 mL	工业废水	/	/	/	6 mL/min	正己烷+二氯甲烷（7∶3），5 mL；MtBE，5 mL；甲醇，5 mL	DMSO，0.2 mL	〔54〕
HLB	遗传毒性	500 mg，6 mL	地上水，地表水	1.2 μm	62 L	3	5~10 mL/min	丙酮，20 mL	DMSO，100 μL	〔55〕
HLB	内分泌干扰毒性		工业废水	0.7 μm	1 L	/	/	正己烷；二氯甲烷；甲醇	DMSO，1 mL	〔56〕
HLB	内分泌干扰毒性、遗传毒性、致癌毒性	12 mg	市政污水	0.45 μm	/	/	10 mL/min	丙酮+二氯甲烷，10 mL	DMSO，1 mL	〔41〕
HLB	内分泌干扰毒性、致癌毒性	200 mg，6 mL	地表水	/	500 mL	/	1 mL/min	二氯甲烷+正己烷（1∶1），10 mL	正己烷，100 μL	〔57〕
HLB	遗传毒性、内分泌干扰毒性、氧化应激毒性	1 g	饮用水	/	5 L	/	/	甲醇，10 mL	甲醇，1 mL	〔58〕
HLB	内分泌干扰毒性、致癌毒性、急性毒性	200 mg	工业废水，市政污水	2 μm	1.2 L	3	5 mL/min	甲醇，6 mL	甲醇，1 mL	〔59〕
StrataX	内分泌干扰毒性	500 mg，6 mL	地表水	0.8 μm	1 L	3	10 mL/min	甲醇，5 mL；甲醇（0.1%氨水），5 mL	5%甲醇，1 mL	〔60〕
StrataX	内分泌干扰毒性	200 mg	饮用水，地表水，市政污水	/	污水：200 mL，地表水：1 000 mL，饮用水：2 000 mL	2	7~10 mL/min	甲醇，3 mL；乙腈，3 mL；丙酮，3 mL	甲醇，1 mL	〔42〕
XAD	遗传毒性	XAD-4，XAD-8	地表水	0.45 μm	15 L	/	/	丙酮，20 mL	DMSO	〔61〕
XAD	细胞毒性、遗传毒性	110 mL XAD-2，XAD-8	市政污水	1.6 μm	13 L	＜2	/	乙酸乙酯，400 mL	DMSO，130 μL	〔44〕
XAD	细胞毒性	55 mL XAD-2	市政污水，工业废水	/	/	1	/	乙酸乙酯	DMSO	〔62〕
XAD	遗传毒性、细胞毒性	30 mL XAD-2，XAD-8	饮用水	0.45 μm	1 L	＜2		乙酸乙酯，200 mL	DMSO，10 μL	〔63〕
XAD	遗传毒性	40 mL XAD-2	地表水，饮用水	1 μm	/	/	40 mL/min	丙酮，40 mL；丙酮+正己烷（1∶3），120 mL；二氯甲烷，80 mL	DMSO	〔64〕
XAD	细胞毒性	55 mL XAD-2，XAD-8	市政污水	1.6 μm，0.45 μm	2 L	/	/	甲醇；乙酸乙酯；甲醇	DMSO	〔65〕
XAD	遗传毒性	13 mL XAD-2，XAD-8	饮用水	/	20 L	/	/	丙酮	/	〔66〕
XAD	细胞毒性、遗传毒性、致突变性、胚胎毒性、内分泌干扰毒性	XAD-4，XAD-7	市政污水，工业废水	0.45 μm	20 L	2	17 mL/min	甲醇，50 mL；丙酮，50 mL	乙醇+DMSO（1∶2），2 mL	〔46〕

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