石墨化炭黑去除水产养殖尾水中恩诺沙星残留的研究

doi:10.3785/j.issn.1008-9209.2023.07.191

浙江大学学报（农业与生命科学版）

2024, Vol. 50

Issue (5): 785-795 DOI: 10.3785/j.issn.1008-9209.2023.07.191

资源利用与环境保护

石墨化炭黑去除水产养殖尾水中恩诺沙星残留的研究

李梦妍¹(

),齐梦钰^2,³,吴佳龙¹,李铁军²,胡红美²(

),张小宁¹(

)

^1.资源昆虫高效养殖与利用全国重点实验室/西南大学蚕桑纺织与生物质科学学院，重庆 400715
^2.浙江省海洋水产研究所，浙江省海洋渔业资源可持续利用技术研究重点实验室，浙江舟山 316021
^3.浙江海洋大学水产学院，浙江舟山 316022

Removal of enrofloxacin residues from aquaculture tailwater by graphitized carbon black

Mengyan LI¹(

),Mengyu QI^2,³,Jialong WU¹,Tiejun LI²,Hongmei HU²(

),Xiaoning ZHANG¹(

)

^1.State Key Laboratory of Resource Insects/College of Sericulture, Textile and Biomass Sciences, Southwest University, Chongqing 400715, China
^2.Key Laboratory of Sustainable Utilization of Technology Research for Fisheries Resources of Zhejiang Province, Zhejiang Marine Fisheries Research Institute, Zhoushan 316021, Zhejiang, China
^3.Institute of Marine and Fisheries, Zhejiang Ocean University, Zhoushan 316021, Zhejiang, China

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摘要：

本研究探究并评价了石墨化炭黑（graphitized carbon black, GCB）吸附去除水产养殖环境中恩诺沙星（enrofloxacin, ENR）的能力。通过扫描电子显微镜、傅里叶变换红外光谱仪、拉曼光谱以及Zeta电位对石墨化炭黑进行表征，探讨了pH值、吸附温度（T）、恩诺沙星初始质量浓度（C₀）、吸附时间（t）对石墨化炭黑吸附恩诺沙星的影响。同时，从吸附热力学和吸附动力学等方面探究了石墨化炭黑对恩诺沙星的吸附机制。结果表明，石墨化炭黑对恩诺沙星具有良好的吸附能力，吸附过程符合伪二级动力学模型和弗罗因德利希（Freundlich）吸附等温模型。在 $p H$ =7、 $C 0$ =200 mg/L、 $T$ =35 ℃的条件下，石墨化炭黑对溶液中恩诺沙星的吸附能力最强，最大吸附量可达74.43 mg/g。此外，石墨化炭黑对实际加标养殖淡水和加标养殖海水中恩诺沙星残留具有较好的吸附去除能力，单位吸附量分别为（32.47±0.99）、（31.84±1.46） mg/g。综上所述，石墨化炭黑具有去除实际水产养殖尾水中恩诺沙星的应用潜力。

关键词： 石墨化炭黑; 恩诺沙星; 吸附; 去除; 水产养殖环境

Abstract:

This study explored and evaluated the adsorption capacity of graphitized carbon black (GCB) to remove enrofloxacin (ENR) in an aquaculture environment. GCB was characterized by scanning electron microscope, Fourier transform infrared spectrometer, Raman spectrum and Zeta potential. Additionally, the effects of pH value, adsorption temperature (T), initial concentration of ENR (C₀) and adsorption time (t) on the adsorption of ENR by GCB were determined. Meanwhile, the adsorption thermodynamics and adsorption kinetics of ENR by GCB were explored to reveal its adsorption mechanisms. The results showed that GCB had good adsorption performance to ENR, which can be described by the pseudo-second-order kinetic model and the Freundlich adsorption isotherm model. Under the conditions of $p H$ =7, $C 0$ =200 mg/L and $T$ =35 ℃, GCB had the strongest adsorption capacity for ENR in solution, and the maximum adsorption quantity could reach 74.43 mg/g. Furthermore, it was found that GCB demonstrated good adsorption quantity on ENR residues in actual spiked cultural freshwater and spiked cultural seawater, and the unit adsorption quantities were (32.47±0.99) mg/g and (31.84±1.46) mg/g, respectively. In conclusion, GCB has the potential to remove ENR from real aquaculture tailwater.

Key words: graphitized carbon black enrofloxacin adsorption removal aquaculture environment

收稿日期: 2023-07-19 出版日期: 2024-10-31

CLC:

X52

基金资助: 重庆市自然科学基金项目(CSTB2024NSCQ-MSX0515);重庆市商务委员会2024年茧丝绸发展项目(20240523172126600);国家自然科学基金项目(31800430);浙江省舟山市科技项目(2024C31044)

通讯作者: 胡红美,张小宁 E-mail: lm20011219@email.swu.edu.cn;huhm@zju.edu.cn;xzhang@swu.edu.cn

作者简介: 李梦妍（https://orcid.org/0009-0000-7608-8211），E-mail：lm20011219@email.swu.edu.cn

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引用本文:

李梦妍,齐梦钰,吴佳龙,李铁军,胡红美,张小宁. 石墨化炭黑去除水产养殖尾水中恩诺沙星残留的研究[J]. 浙江大学学报（农业与生命科学版）, 2024, 50(5): 785-795.

Mengyan LI,Mengyu QI,Jialong WU,Tiejun LI,Hongmei HU,Xiaoning ZHANG. Removal of enrofloxacin residues from aquaculture tailwater by graphitized carbon black. Journal of Zhejiang University (Agriculture and Life Sciences), 2024, 50(5): 785-795.

链接本文:

https://www.zjujournals.com/agr/CN/10.3785/j.issn.1008-9209.2023.07.191 或 https://www.zjujournals.com/agr/CN/Y2024/V50/I5/785

表1 恩诺沙星质谱参数

图1 石墨化炭黑的扫描电子显微镜图及其粒径频率分布图

图2 石墨化炭黑吸附恩诺沙星前后的FTIR（A）和石墨化炭黑的拉曼光谱（B）

图3 溶液pH值对石墨化炭黑对恩诺沙星吸附能力的影响以及不同pH值下石墨化炭黑的Zeta电位

图4 不同的吸附温度和恩诺沙星初始质量浓度对石墨化炭黑吸附恩诺沙星的影响

表2 本研究与已报道的碳基吸附剂对恩诺沙星的吸附能力的比较

T/℃	Langmuir吸附等温线 Langmuir adsorption isotherm			Freundlich吸附等温线 Freundlich adsorption isotherm			吉布斯自由能 $? G$ /(kJ/mol)
T/℃	$q m$ /(mg/g)	$K L$ /(L/mg)	$R 2$	$K F$ /((L^1/ⁿ ?mg^(1－1/ⁿ⁾)/g)	$1 / n$	$R 2$	吉布斯自由能 $? G$ /(kJ/mol)
35	75.24	0.205 3	0.697 6	38.71	0.130 4	0.976 8	－0.050 9
25	65.59	1.455 2	0.736 8	37.87	0.127 7	0.986 2	－0.051 5
15	67.10	0.341 1	0.619 6	32.57	0.147 4	0.976 5	－0.061 5

表3 石墨化炭黑在不同吸附温度下吸附恩诺沙星的Langmuir、Freundlich吸附等温线参数

图5 不同吸附温度下拟合得到的Langmuir、Freundlich吸附等温线图中实线表示拟合的Langmuir吸附等温线，虚线表示拟合的Freundlich吸附等温线。

图6 不同恩诺沙星初始质量浓度下石墨化炭黑吸附恩诺沙星的伪一级（A）、伪二级（B）动力学模型和颗粒内扩散模型（C）拟合曲线图C中，实线表示颗粒内扩散模型连续性的分段吸附过程，虚线表示颗粒内扩散模型拟合曲线。

$C 0 /$ (mg/L)	伪一级动力学模型 Pseudo-first-order kinetic model			伪二级动力学模型 Pseudo-second-order kinetic model			颗粒内扩散模型 Intra-particle diffusion model
$C 0 /$ (mg/L)	$k 1$ /min^－1	$q e /$ (mg/g)	$R 2$	$k 2 /$ (g/(mg?min))	$q e$ /(mg/g)	$R 2$	$k i$ /(mg/(g?min^1/2))	$C$ /(mg/g)	$R 2$
30	0.187 0	43.89	0.920 9	0.003 5	45.75	0.999 9	0.384 8	35	0.293 4
40	0.223 0	48.02	0.923 5	0.007 4	49.36	1.000 0	0.272 1	42	0.459 9
50	0.248 0	53.28	0.920 4	0.005 2	54.98	0.999 9	0.294 8	48	0.545 5

表4 不同恩诺沙星初始质量浓度下石墨化炭黑吸附恩诺沙星的伪一级、伪二级动力学模型和颗粒内扩散模型参数

图7 NaCl质量浓度对石墨化炭黑对恩诺沙星吸附能力的影响

图8 GCB对HEK-293细胞的毒性作用短栅上图为培养第1、2、3天时各组细胞形态。“ns”表示差异无统计学意义。

图9 3种实际加标水样中石墨化炭黑对恩诺沙星的去除效果**表示在P＜0.01水平差异有统计学意义（双样本t检验），“ns”表示差异无统计学意义。

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