不同结构表面活性剂改性黏土对海洋卡盾藻的去除作用研究
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摘要
海洋卡盾藻赤潮在我国沿海频繁爆发,给海产养殖业带来严重的经济损失,已成为我国南方重要的有害赤潮种类。赤潮治理的方法有很多种,各自存在的弊端使得其在实际应用中受到限制。采用改性黏土可以在提高黏土对藻细胞的去除率的同时,降低黏土的用量。
本文在实验室条件下,采用结构不同的表面活性剂(单链季铵盐、单链季磷盐、吉米奇表面活性剂)改性黏土,通过比较不同改性黏土的除藻效能与改性剂结构间的关系,揭示影响改性黏土除藻活性的因素,以便为筛选新的除藻剂提供参考。同时,论文以模式生物斑马鱼(Brachydanio rerio)及广东常见经济水产品种凡纳滨对虾(Litopenaeus vannamei)为生物毒性研究对象,考查了初筛改性黏土的生物毒性,分析了改性粘土的播散对水体中氮营养盐的可能影响,以了解改性黏土对水体环境的影响,为改性黏土的实际应用提供必要数据。
研究结果表明,链长为十四烷基的季铵盐改性黏土的除藻效果最好,其次为十二烷基和十烷基,而十六烷基较差；季铵(磷)盐取代基团对改性黏土除藻效果的影响不大。十四烷基三丁基溴化磷改性黏土和双十四烷基二甲基乙基溴化铵改性黏土的除藻效果最好,对海洋卡盾藻的120 h半抑制质量浓度分别为6.11mg／L和6.13 mg／L。毒性试验表明,这2种改性黏土对斑马鱼的毒性均较低,质量浓度为10-100 mg／L时,96h后斑马鱼的存活率均为100%。改性黏土对蒙古裸腹蚤有一定毒性,其中十四烷基三丁基溴化磷改性黏土24 h的LCso远超过100mg／L,双十四烷基二甲基乙基溴化铵改性黏土的LC50为9.37 mg／L。因此,十四烷基三丁基溴化磷改性黏土的毒性更低,有望成为赤潮治理的潜在除藻剂。
四种不同结构的吉米奇表面活性剂对海洋卡盾藻均具有良好的去除效果,其中乙撑基双(十二烷基二甲基溴化铵)(Ethylene bis(dodecyl dimethyl ammonium bromide), EDAB)对海洋卡盾藻的去除作用最优,对海洋卡盾藻的120 h半抑制浓度为0.42 mg／L；EDAB与天然黏土的复配实验显示,黏土与EDAB复配不能增加EDAB对海洋卡盾藻的去除效果；改性黏土的除藻作用具有长效性,并存在最佳配比,改性剂质量百分比为15%时除藻率达到最高,3 mg/L EDAB改性黏土即可有效去除海洋卡盾藻(RE>90%)。生物毒性实验说明,EDAB改性粘土对斑马鱼、幼年凡纳滨对虾和成年凡纳滨的48h LC50分别为25.66 mg／L、12.49mg／L和48.03 mg／L。EDAB改性黏土在有效除藻的同时,可降低水体中可溶性氮盐的水平。这些事实表明,EDAB改性黏土治理赤潮有一定应用前景。
The harmful algal blooms (HABs) frequently occur and result in the serve mortality of fishes and invertebrates, and harm to the cultivation and ecological system in South Chin Sea. It is urgently needed to investigate how to control HABs effectively. However, progress is still slow in developing effective and economic controlling strategies. Many studies on controlling or inhibiting the growth of HABs species have been conducted. Of them, natural clays attracted much attention due to its non-toxic and friendly to environment.
In this paper, to explore the new modified clays with excellent algae removal efficiencies, clays were modified by three kinds of surfactants such single-chain quaternary ammonium salts, single-stranded quarter of phosphate and Gemini surfactants with different structures. The removal efficiencies of the modified clays against Chattonella marina, a typical HABs alga in China were observed. The toxicities of the modified clays with high removal efficiency on Brachydanio rerio, Miona mongolica Daddy and Litopenaeus vannamei were evaluated.
The clays modified by tetradecyl quaternary phosphonium were shown to have the highest removal efficiency, followed by ones with decyl, dodecy and cetyl quaternary phosphonium. The clays modified by tetradecyl quaternary ammonium with different substituent groups such as trimethyl, dimethyl phenmethyl and dimethyl ethide had similar removal efficiency, suggesting less effect of the substituent groups in quaternary ammonium on the algaecide activity of the modified clays. Among the modified clays assayed, the clays with tributyltin bromide tetradecyl phosphonium and two-brominated ethyl dimethyl tetradecyl ammonium had the highest removal efficiency. The EC50120 of the two modified clays against C. marina was only 6.11 mg/L and 6.13 mg/L, respectively, indicating that these two modified clays could remove the algae effectively under low concentrations. Low toxicities of these two modified clays were shown in the acute toxicity tests of B. rerio. None of the B. rerio were killed in 96 h after exposed to the two modified clay in the concentration of 10～100 mg/L. However, some differences in toxicity to M. mongolica were exited between them. The LC50 in 24 h of clay with tributyltin bromide tetradecyl phosphonium against M. mongolica was above 100 mg/L, while the other one was only 9.37 mg/L. Obviously, clay modified by tributyltin bromide tetradecyl phosphonium was less toxic to M. mongolica than that of modified by two-brominated ethyl dimethyl tetradecyl ammonium. Combining the high removal effectiveness on C. marina and low toxicity to B. rerio and M. mongolica, it was reasonable to consider the clay modified by tributyltin bromide tetradecyl phosphonium a potential algaecide with high effectiveness and low toxicity to fishery.
The clays modified by four Gemini surfactants such as ethylene bis(dodecyl dimethyl ammonium chloride) (EDAC), ethylene bis (octadecyl dimethyl ammonium chloride) (EOAC), poly(quaternary ammonium salt)(PQAS) and ethylene bis(dodecyl dimethyl ammonium bromide) (EDAB) were all shown to exhibit high removal efficiencies against C. marina. Among them, the clay modified by EDAB had the highest removal efficiency, with EC50120 of 0.42 mg/L. Simple mixture of EDAB and natural clay did not enhance the removal efficiency of them against C. marina. In contrast, the clay modified by EDAB exhibited higher removal efficiency than EDAB and clay did, with an ideal composition ratio of 15%. At 3 mg/L, removal efficiency of the clay modified with EDAB was above 90%. The LC50 in 48 h of clay with EDAB against B. rerio, juvenile L. vannamei and adult L. vannamei were 25.66, 12.49 and 48.03 mg/L, respectively, suggesting the low toxicity of the modified clay to other aquatic organisms. In addition, EDAB modified clays could reduce the level of soluble nitrogen in water by adsorption. Combining the high removal efficiency on C. marina, low toxicity to B. rerio and L. vannamei, and high adsorption capacity for soluble nitrogen in water, it would probably be reasonable to believe that the clay modified by EDAB should be better a favorable choice to control HABs. However, further studies are awaited to prove the hypothesis we have proposed in the future in an open aqua-ecosystem.
本文在实验室条件下,采用结构不同的表面活性剂(单链季铵盐、单链季磷盐、吉米奇表面活性剂)改性黏土,通过比较不同改性黏土的除藻效能与改性剂结构间的关系,揭示影响改性黏土除藻活性的因素,以便为筛选新的除藻剂提供参考。同时,论文以模式生物斑马鱼(Brachydanio rerio)及广东常见经济水产品种凡纳滨对虾(Litopenaeus vannamei)为生物毒性研究对象,考查了初筛改性黏土的生物毒性,分析了改性粘土的播散对水体中氮营养盐的可能影响,以了解改性黏土对水体环境的影响,为改性黏土的实际应用提供必要数据。
研究结果表明,链长为十四烷基的季铵盐改性黏土的除藻效果最好,其次为十二烷基和十烷基,而十六烷基较差；季铵(磷)盐取代基团对改性黏土除藻效果的影响不大。十四烷基三丁基溴化磷改性黏土和双十四烷基二甲基乙基溴化铵改性黏土的除藻效果最好,对海洋卡盾藻的120 h半抑制质量浓度分别为6.11mg／L和6.13 mg／L。毒性试验表明,这2种改性黏土对斑马鱼的毒性均较低,质量浓度为10-100 mg／L时,96h后斑马鱼的存活率均为100%。改性黏土对蒙古裸腹蚤有一定毒性,其中十四烷基三丁基溴化磷改性黏土24 h的LCso远超过100mg／L,双十四烷基二甲基乙基溴化铵改性黏土的LC50为9.37 mg／L。因此,十四烷基三丁基溴化磷改性黏土的毒性更低,有望成为赤潮治理的潜在除藻剂。
四种不同结构的吉米奇表面活性剂对海洋卡盾藻均具有良好的去除效果,其中乙撑基双(十二烷基二甲基溴化铵)(Ethylene bis(dodecyl dimethyl ammonium bromide), EDAB)对海洋卡盾藻的去除作用最优,对海洋卡盾藻的120 h半抑制浓度为0.42 mg／L；EDAB与天然黏土的复配实验显示,黏土与EDAB复配不能增加EDAB对海洋卡盾藻的去除效果；改性黏土的除藻作用具有长效性,并存在最佳配比,改性剂质量百分比为15%时除藻率达到最高,3 mg/L EDAB改性黏土即可有效去除海洋卡盾藻(RE>90%)。生物毒性实验说明,EDAB改性粘土对斑马鱼、幼年凡纳滨对虾和成年凡纳滨的48h LC50分别为25.66 mg／L、12.49mg／L和48.03 mg／L。EDAB改性黏土在有效除藻的同时,可降低水体中可溶性氮盐的水平。这些事实表明,EDAB改性黏土治理赤潮有一定应用前景。
The harmful algal blooms (HABs) frequently occur and result in the serve mortality of fishes and invertebrates, and harm to the cultivation and ecological system in South Chin Sea. It is urgently needed to investigate how to control HABs effectively. However, progress is still slow in developing effective and economic controlling strategies. Many studies on controlling or inhibiting the growth of HABs species have been conducted. Of them, natural clays attracted much attention due to its non-toxic and friendly to environment.
In this paper, to explore the new modified clays with excellent algae removal efficiencies, clays were modified by three kinds of surfactants such single-chain quaternary ammonium salts, single-stranded quarter of phosphate and Gemini surfactants with different structures. The removal efficiencies of the modified clays against Chattonella marina, a typical HABs alga in China were observed. The toxicities of the modified clays with high removal efficiency on Brachydanio rerio, Miona mongolica Daddy and Litopenaeus vannamei were evaluated.
The clays modified by tetradecyl quaternary phosphonium were shown to have the highest removal efficiency, followed by ones with decyl, dodecy and cetyl quaternary phosphonium. The clays modified by tetradecyl quaternary ammonium with different substituent groups such as trimethyl, dimethyl phenmethyl and dimethyl ethide had similar removal efficiency, suggesting less effect of the substituent groups in quaternary ammonium on the algaecide activity of the modified clays. Among the modified clays assayed, the clays with tributyltin bromide tetradecyl phosphonium and two-brominated ethyl dimethyl tetradecyl ammonium had the highest removal efficiency. The EC50120 of the two modified clays against C. marina was only 6.11 mg/L and 6.13 mg/L, respectively, indicating that these two modified clays could remove the algae effectively under low concentrations. Low toxicities of these two modified clays were shown in the acute toxicity tests of B. rerio. None of the B. rerio were killed in 96 h after exposed to the two modified clay in the concentration of 10～100 mg/L. However, some differences in toxicity to M. mongolica were exited between them. The LC50 in 24 h of clay with tributyltin bromide tetradecyl phosphonium against M. mongolica was above 100 mg/L, while the other one was only 9.37 mg/L. Obviously, clay modified by tributyltin bromide tetradecyl phosphonium was less toxic to M. mongolica than that of modified by two-brominated ethyl dimethyl tetradecyl ammonium. Combining the high removal effectiveness on C. marina and low toxicity to B. rerio and M. mongolica, it was reasonable to consider the clay modified by tributyltin bromide tetradecyl phosphonium a potential algaecide with high effectiveness and low toxicity to fishery.
The clays modified by four Gemini surfactants such as ethylene bis(dodecyl dimethyl ammonium chloride) (EDAC), ethylene bis (octadecyl dimethyl ammonium chloride) (EOAC), poly(quaternary ammonium salt)(PQAS) and ethylene bis(dodecyl dimethyl ammonium bromide) (EDAB) were all shown to exhibit high removal efficiencies against C. marina. Among them, the clay modified by EDAB had the highest removal efficiency, with EC50120 of 0.42 mg/L. Simple mixture of EDAB and natural clay did not enhance the removal efficiency of them against C. marina. In contrast, the clay modified by EDAB exhibited higher removal efficiency than EDAB and clay did, with an ideal composition ratio of 15%. At 3 mg/L, removal efficiency of the clay modified with EDAB was above 90%. The LC50 in 48 h of clay with EDAB against B. rerio, juvenile L. vannamei and adult L. vannamei were 25.66, 12.49 and 48.03 mg/L, respectively, suggesting the low toxicity of the modified clay to other aquatic organisms. In addition, EDAB modified clays could reduce the level of soluble nitrogen in water by adsorption. Combining the high removal efficiency on C. marina, low toxicity to B. rerio and L. vannamei, and high adsorption capacity for soluble nitrogen in water, it would probably be reasonable to believe that the clay modified by EDAB should be better a favorable choice to control HABs. However, further studies are awaited to prove the hypothesis we have proposed in the future in an open aqua-ecosystem.
引文
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