基于离子印迹硅胶方法的土壤镉生物有效性模拟研究
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摘要
随着国民经济的迅速发展,土壤重金属污染问题日益凸现,对生态环境、食品安全、人体健康、农业可持续发展造成严重危害,引起了广泛的社会关注。目前多以重金属总量作为土壤重金属污染评价基准,评价结果往往有背于实际情况,众多的研究成果表明,仅以土壤中重金属总量并不能很好地预测评估土壤重金属的生物有效性及其环境效应,更大程度上由其形态分布决定。形态不同,其产生的环境效应和生物效应也不同。众所周知,游离态的重金属与重金属的毒害作用有直接关系,目前能够直接提取土壤中游离态的重金属浓度的方法比较少见。因此,本文利用二乙烯三胺基丙基三甲氧基硅烷、3-硫氰基丙基三乙氧基硅烷具有对Cd2+有专性吸附作用的特性,以正硅酸乙酯为前驱体,应用印迹溶胶-凝胶法,制备了2种对镉离子有选择性吸附的功能化离子印迹硅胶材料,通过对其合成条件及方式进行分析,对其物理以及化学特性进行研究,表明离子印迹硅胶可以以试剂盒为载体对镉进行生物有效性预测。并与化学提取法、离子选择电极法等相比较,通过盆栽试验,考查不同影响因素下离子印迹硅胶测量土壤中重金属镉离子生物有效性的准确性,建立离子印迹硅胶测量技术评估土壤中重金属生物有效性的方法,主要结论如下：
(1)按照印迹溶胶凝胶法,以镉离子为模板离子,以含有配位基团胺基和硫氰基的2种硅烷作为功能单体,通过配位作用结合形成螯合化合物,去除重金属离子获得了与金属离子相对应的具有三维孔穴结构的胺基功能化和硫氰基功能化印迹硅胶,形成的三维孔穴对重金属离子具有特异选择性；通过IR、SEM、TGA-DTA和N2吸附试验研究了2种功能化印迹硅胶的结构和性能。IR和TGA-DTA结果表明,功能化基团成功接枝到硅胶表面；SEM和N2吸附结果表明,所得到的功能化印迹硅胶表面粗糙,BET增大,通过印迹技术在硅胶表面确实形成了印迹空穴。利用静态吸附试验结果表明,硫氰基功能化和胺基功能化镉离子印迹硅胶材料的饱和吸附容量分别为72.8和77.2mg·g-1；2种印迹硅胶材料的pH值适用范围为4-8;2种印迹硅胶材料对镉离子20min就能达到吸附平衡；2种印迹硅胶材料对镉离子均有较好的选择性吸附能力；2种印迹硅胶材料对镉离子均有较好的再生能力,可以多次循环使用。吸附机理研究表明,硫氰基功能化镉离子印迹硅胶材料对Cd2+离子的吸附模型更符合Redlieh-Peterson吸附模型,胺基功能化镉离子印迹硅胶材料对Cd2+离子的吸附模型更符合Langmuir吸附模型；吸附动力学研究表明,准二级动力学方程对2种镉离子印迹硅胶材吸附Cd2+离子的动力拟合最佳；吸附热力学研究表明,2种镉离子印迹硅胶材的△G°均为负值,说明Cd2+离子的吸附的过程是自发过程,△H°均为正值,Cd2+的吸附过程是吸热的,升高温度有助于吸附的进行,△S°均为正值,显示该过程为熵增过程,混乱度是增加的。
(2)以不同孔径的PES膜作为扩散膜,以试剂盒为载体分别以硫氰基功能化和胺基功能化镉离子印迹硅胶作为结合膜,经筛选,Cd2+离子在0.22μm的PES膜中扩散系数比在0.45μm的PES膜中扩散系数小一个数量级,0.22μm的PES膜可以起到控制Cd2+离子扩散的作用,故采用0.22μm的PES膜作为离子印迹硅胶试剂盒的扩散膜；当印迹硅胶与预凝胶溶液的固液比为4g/40mL时,结合膜凝胶对Cd2+离子吸附量达到最佳。
(3)在0.01mol·L-1NaNO3溶液中,胺基离子印迹硅胶试剂盒能够准确的提取水溶液中游离镉离子的浓度；而硫氰基离子印迹硅胶试剂盒的提取值则偏低；在含有不同量EDTA的Cd2+溶液中,胺基离子印迹硅胶试剂盒仍然可以准确的定量提取水溶液中游离镉离子的浓度,其提取值与溶液中游离镉离子的理论值之间没有显著性的差异；而硫氰基离子印迹硅胶试剂盒所得到的提取值明显小于理论值,上述结果进一步表明,胺基离子印迹硅胶试剂盒可以准确的提取溶液中游离Cd2+离子的浓度,硫氰基离子印迹硅胶试剂盒的提取值偏低,不能用于定量提取溶液中游离Cd2+离子的浓度；当溶液的pH值在5-8、离子强度在0.005-0.1m01·L-1之间变化时,pH值和离子强度将不会影响胺基离子印迹硅胶试剂盒对溶液中游离Cd2+离子的准确提取；比较了胺基离子印迹硅胶试剂盒和Cd-ISE对在不同水样中游离Cd2+离子的测量,结果表明,胺基离子印迹硅胶试剂盒和Cd-ISE对游离Cd2+离子的测量是等效的,而胺基离子印迹硅胶试剂盒的检出浓度低于Cd-ISE,其灵敏度高于Cd-ISE.
(4)将胺基离子印迹硅胶试剂盒应用于提取土壤中游离Cd2+离子,结果表明,在5个含有不同水平Cd2+离子的土壤中,胺基离子印迹硅胶试剂盒和Cd-ISE对游离Cd2+离子的测量是等效的；当土壤含水量在80-150%范围内时,胺基离子印迹硅胶试剂盒提取土壤游离态Cd2+的准确性不受影响；胺基离子印迹硅胶试剂盒提取游离态Cd2+受到土壤pH值强烈的影响,所提取游离态Cd2+的浓度随着土壤pH值降低而升高；与土壤溶液和MgCl2提取法相比较,离子印迹硅胶提取的游离态镉含量与黑麦草吸收金属含量的相关性明显优于其它的形态分析方法。结果表明,胺基离子印迹硅胶试剂盒能够成为一种提取土壤中游离态Cd2+的新方法,其预测土壤中镉生物有效性可行并且有效。
综上,离子印迹硅胶能够成为一种定量提取土壤中游离态Cd2+离子的新工具,为评估重金属的环境与健康风险提供有力的技术支持。
With the rapid development of the national economy, heavy metal pollution problems have become increasing apparently, have caused serious harm for the ecological environment, food safety, human health and sustainable development of agriculture, and have obtained widespread concern in the community. At present, the total concentrations of heavy metals usually are used as the evaluation criteria of heavy metal pollution in soils, however, the evaluation results are often incompatible with the actual situation. Many of the research results show that the bioavailability of heavy metals and its environmental effect can not be predicted by the total concentrations of heavy metals in soil, to a greater extent determined by the speciation distribution of heavy metals. The different speciation of heavy metals can produce the different environmental and biological effects. As we all know, free state of heavy metals have a direct relationship with its toxic effects, however, the methods which can directly measure free state of heavy metals in soil are relatively low. In this paper, cadmium as a representative of toxic heavy metals, a new diffusive gradients in thin films (imprinted functionalized silica gel) device were developed to measure free state of Cd(II) in soil by the diffusion layer and binding agent. Performance of imprinted functionalized silica gel device was studied. The effects of pH and ionic strength on the validation of imprinted functionalized silica gel device were also studied. Comparison of imprinted functionalized silica gel device and ion-selective electrodes for the measurement of free Cd(II) was assessed. The concentrations of free Cd(II) in different samples by imprinted functionalized silica gel device were measured. The objective of the paper will provide a simple and reliable tool for measurement of free Cd2+in soils, and a potential technical support for the assessing the environmental and health risks of heavy metals. Conclusions are as follows:
1. A simple procedure was developed to synthesize Cd(II)-imprinted thiocyanato-functionalized silica gel (SCN/IIP) and Cd(Ⅱ)-imprinted amino-functionalized silica gel (N3/IIP) sorbents by combining a surface molecular imprinting technique with a sol-gel process. The maximum static adsorption capacities of SCN/IIP and N3/IIP were72.8T77.2mg·g-1, respectively. Two sorbents offered a fast kinetics for the adsorption of Cd(Ⅱ) for20min, had a substantial binding capacity in the range of pH4-8, could be used repeatedly, and were found to adsorb selectively Cd2+in the presence of Co(Ⅱ), Ni(Ⅱ), Zn(Ⅱ), Pb(Ⅱ) and Cu(Ⅱ) interferences in the same medium. The equilibrium data of SCN/IIP fitted perfectly with Redlieh-Peterson isotherm model. The equilibrium data of N3/IIP fitted perfectly with Langmuir isotherm model. Kinetic studies of SCN/IIP and N3/IIP indicated that the adsorption for Cd(II) by two sorbents followed a pseudo-second-order model. Various thermodynamic parameters such as△G0,△H0and△S0were evaluated. Negative values of△G0of SCN/IIP and N3/IIP indicated that the adsorption process was spontaneous. The positive standard enthalpy change of two sorbents suggested that the adsorption of Cd(II) by sorbents was endothermic. The positive values of△S0exhibited that the randomness increased with the adsorption of Cd(Ⅱ) on two sorbents.
2. The diffusion coefficients of Cd(II) ions through PES membranes with different pore diameters (0.22and0.45μm) were8.5×10-6和2.6×10-5cm2s-1, respectively. The PES membrane with0.22μm of pore diameter was suitable as the diffusion layer.
3. Two imprinted functionalized silica gel devices using SCN/IIP and N3/IIP as the binding agents and PES membrane with0.22μm of pore diameter as the diffusive layer, namely, PES-SCN/IIP-imprinted functionalized silica gel and PES-Nj/IIP-imprinted functionalized silica gel, had been systemically investigated. The ratios of Ci/Cbulk for free Cd(II) in NaNO3solution of0.01mol·L-1by PES-SCN/-imprinted functionalized silica gel and PES-N3/-imprinted functionalized silica gel were0.9869±0.0492and0.6246±0.0678, respectively. PES-SCN/-imprinted functionalized silica gel and PES-N3/-imprinted functionalized silica gel were deployed in synthetic solution with the different molar ratios of Cd(II)ions/EDTA of4:4,4:3,4:2and4:1. The ratios of Ci/Cbuik for free Cd(II) by PES-SCN/-imprinted functionalized silica gel were0,14.95±1.21,28.91±1.73and42.84±1.92%, respectively. There was a noted difference between theoretical and experimental values. The ratio of Ci/Cbuik for free Cd(II) by PES-N3/-imprinted functionalized silica gel were0,24.63±1.42,49.25±1.96and75.49±2.48%, respectively and were very close to the theoretical percentages of free metals in the solutions. The PES-N3/-imprinted functionalized silica gel for can accurately determine free Cd(II) in synthetic solution, while the measured value by PES-SCN/-imprinted functionalized silica gel was low. The PES-N3/-imprinted functionalized silica gel had a substantial binding capacity at pH5-8and concentrations of competitive Na+up to0.1mol·L-1. The measurements of PES-N3/-imprinted functionalized silica gel and Cd(II) ion selective electrode for free Cd(II) in river water were equivalent.
4. The PES-N3/-imprinted functionalized silica gel for can accurately determine free Cd(II) in soil. The measurements of free Cd(II) by PES-N3/-imprinted functionalized silica gel was feasible. Compared with chemical extraction method, PES-N3/-imprinted functionalized silica gel device can be used as a new tool for measurement of free Cd(II).The extraction of Imprinted functionalized silica gel for free Cd(II) is superior to other methods of morphological analysis. The results showed that the Imprinted functionalized silica gel can become a kind of new method of extracting ree Cd(II) in soil.
In summary, imprinted functionalized silica gel can used as a new tool for the quantitative measurement and sampling of free Cd(II) in soil and can provide strong technical support for assessing the environmental and health risks of heavy metals.
(1)按照印迹溶胶凝胶法,以镉离子为模板离子,以含有配位基团胺基和硫氰基的2种硅烷作为功能单体,通过配位作用结合形成螯合化合物,去除重金属离子获得了与金属离子相对应的具有三维孔穴结构的胺基功能化和硫氰基功能化印迹硅胶,形成的三维孔穴对重金属离子具有特异选择性；通过IR、SEM、TGA-DTA和N2吸附试验研究了2种功能化印迹硅胶的结构和性能。IR和TGA-DTA结果表明,功能化基团成功接枝到硅胶表面；SEM和N2吸附结果表明,所得到的功能化印迹硅胶表面粗糙,BET增大,通过印迹技术在硅胶表面确实形成了印迹空穴。利用静态吸附试验结果表明,硫氰基功能化和胺基功能化镉离子印迹硅胶材料的饱和吸附容量分别为72.8和77.2mg·g-1；2种印迹硅胶材料的pH值适用范围为4-8;2种印迹硅胶材料对镉离子20min就能达到吸附平衡；2种印迹硅胶材料对镉离子均有较好的选择性吸附能力；2种印迹硅胶材料对镉离子均有较好的再生能力,可以多次循环使用。吸附机理研究表明,硫氰基功能化镉离子印迹硅胶材料对Cd2+离子的吸附模型更符合Redlieh-Peterson吸附模型,胺基功能化镉离子印迹硅胶材料对Cd2+离子的吸附模型更符合Langmuir吸附模型；吸附动力学研究表明,准二级动力学方程对2种镉离子印迹硅胶材吸附Cd2+离子的动力拟合最佳；吸附热力学研究表明,2种镉离子印迹硅胶材的△G°均为负值,说明Cd2+离子的吸附的过程是自发过程,△H°均为正值,Cd2+的吸附过程是吸热的,升高温度有助于吸附的进行,△S°均为正值,显示该过程为熵增过程,混乱度是增加的。
(2)以不同孔径的PES膜作为扩散膜,以试剂盒为载体分别以硫氰基功能化和胺基功能化镉离子印迹硅胶作为结合膜,经筛选,Cd2+离子在0.22μm的PES膜中扩散系数比在0.45μm的PES膜中扩散系数小一个数量级,0.22μm的PES膜可以起到控制Cd2+离子扩散的作用,故采用0.22μm的PES膜作为离子印迹硅胶试剂盒的扩散膜；当印迹硅胶与预凝胶溶液的固液比为4g/40mL时,结合膜凝胶对Cd2+离子吸附量达到最佳。
(3)在0.01mol·L-1NaNO3溶液中,胺基离子印迹硅胶试剂盒能够准确的提取水溶液中游离镉离子的浓度；而硫氰基离子印迹硅胶试剂盒的提取值则偏低；在含有不同量EDTA的Cd2+溶液中,胺基离子印迹硅胶试剂盒仍然可以准确的定量提取水溶液中游离镉离子的浓度,其提取值与溶液中游离镉离子的理论值之间没有显著性的差异；而硫氰基离子印迹硅胶试剂盒所得到的提取值明显小于理论值,上述结果进一步表明,胺基离子印迹硅胶试剂盒可以准确的提取溶液中游离Cd2+离子的浓度,硫氰基离子印迹硅胶试剂盒的提取值偏低,不能用于定量提取溶液中游离Cd2+离子的浓度；当溶液的pH值在5-8、离子强度在0.005-0.1m01·L-1之间变化时,pH值和离子强度将不会影响胺基离子印迹硅胶试剂盒对溶液中游离Cd2+离子的准确提取；比较了胺基离子印迹硅胶试剂盒和Cd-ISE对在不同水样中游离Cd2+离子的测量,结果表明,胺基离子印迹硅胶试剂盒和Cd-ISE对游离Cd2+离子的测量是等效的,而胺基离子印迹硅胶试剂盒的检出浓度低于Cd-ISE,其灵敏度高于Cd-ISE.
(4)将胺基离子印迹硅胶试剂盒应用于提取土壤中游离Cd2+离子,结果表明,在5个含有不同水平Cd2+离子的土壤中,胺基离子印迹硅胶试剂盒和Cd-ISE对游离Cd2+离子的测量是等效的；当土壤含水量在80-150%范围内时,胺基离子印迹硅胶试剂盒提取土壤游离态Cd2+的准确性不受影响；胺基离子印迹硅胶试剂盒提取游离态Cd2+受到土壤pH值强烈的影响,所提取游离态Cd2+的浓度随着土壤pH值降低而升高；与土壤溶液和MgCl2提取法相比较,离子印迹硅胶提取的游离态镉含量与黑麦草吸收金属含量的相关性明显优于其它的形态分析方法。结果表明,胺基离子印迹硅胶试剂盒能够成为一种提取土壤中游离态Cd2+的新方法,其预测土壤中镉生物有效性可行并且有效。
综上,离子印迹硅胶能够成为一种定量提取土壤中游离态Cd2+离子的新工具,为评估重金属的环境与健康风险提供有力的技术支持。
With the rapid development of the national economy, heavy metal pollution problems have become increasing apparently, have caused serious harm for the ecological environment, food safety, human health and sustainable development of agriculture, and have obtained widespread concern in the community. At present, the total concentrations of heavy metals usually are used as the evaluation criteria of heavy metal pollution in soils, however, the evaluation results are often incompatible with the actual situation. Many of the research results show that the bioavailability of heavy metals and its environmental effect can not be predicted by the total concentrations of heavy metals in soil, to a greater extent determined by the speciation distribution of heavy metals. The different speciation of heavy metals can produce the different environmental and biological effects. As we all know, free state of heavy metals have a direct relationship with its toxic effects, however, the methods which can directly measure free state of heavy metals in soil are relatively low. In this paper, cadmium as a representative of toxic heavy metals, a new diffusive gradients in thin films (imprinted functionalized silica gel) device were developed to measure free state of Cd(II) in soil by the diffusion layer and binding agent. Performance of imprinted functionalized silica gel device was studied. The effects of pH and ionic strength on the validation of imprinted functionalized silica gel device were also studied. Comparison of imprinted functionalized silica gel device and ion-selective electrodes for the measurement of free Cd(II) was assessed. The concentrations of free Cd(II) in different samples by imprinted functionalized silica gel device were measured. The objective of the paper will provide a simple and reliable tool for measurement of free Cd2+in soils, and a potential technical support for the assessing the environmental and health risks of heavy metals. Conclusions are as follows:
1. A simple procedure was developed to synthesize Cd(II)-imprinted thiocyanato-functionalized silica gel (SCN/IIP) and Cd(Ⅱ)-imprinted amino-functionalized silica gel (N3/IIP) sorbents by combining a surface molecular imprinting technique with a sol-gel process. The maximum static adsorption capacities of SCN/IIP and N3/IIP were72.8T77.2mg·g-1, respectively. Two sorbents offered a fast kinetics for the adsorption of Cd(Ⅱ) for20min, had a substantial binding capacity in the range of pH4-8, could be used repeatedly, and were found to adsorb selectively Cd2+in the presence of Co(Ⅱ), Ni(Ⅱ), Zn(Ⅱ), Pb(Ⅱ) and Cu(Ⅱ) interferences in the same medium. The equilibrium data of SCN/IIP fitted perfectly with Redlieh-Peterson isotherm model. The equilibrium data of N3/IIP fitted perfectly with Langmuir isotherm model. Kinetic studies of SCN/IIP and N3/IIP indicated that the adsorption for Cd(II) by two sorbents followed a pseudo-second-order model. Various thermodynamic parameters such as△G0,△H0and△S0were evaluated. Negative values of△G0of SCN/IIP and N3/IIP indicated that the adsorption process was spontaneous. The positive standard enthalpy change of two sorbents suggested that the adsorption of Cd(II) by sorbents was endothermic. The positive values of△S0exhibited that the randomness increased with the adsorption of Cd(Ⅱ) on two sorbents.
2. The diffusion coefficients of Cd(II) ions through PES membranes with different pore diameters (0.22and0.45μm) were8.5×10-6和2.6×10-5cm2s-1, respectively. The PES membrane with0.22μm of pore diameter was suitable as the diffusion layer.
3. Two imprinted functionalized silica gel devices using SCN/IIP and N3/IIP as the binding agents and PES membrane with0.22μm of pore diameter as the diffusive layer, namely, PES-SCN/IIP-imprinted functionalized silica gel and PES-Nj/IIP-imprinted functionalized silica gel, had been systemically investigated. The ratios of Ci/Cbulk for free Cd(II) in NaNO3solution of0.01mol·L-1by PES-SCN/-imprinted functionalized silica gel and PES-N3/-imprinted functionalized silica gel were0.9869±0.0492and0.6246±0.0678, respectively. PES-SCN/-imprinted functionalized silica gel and PES-N3/-imprinted functionalized silica gel were deployed in synthetic solution with the different molar ratios of Cd(II)ions/EDTA of4:4,4:3,4:2and4:1. The ratios of Ci/Cbuik for free Cd(II) by PES-SCN/-imprinted functionalized silica gel were0,14.95±1.21,28.91±1.73and42.84±1.92%, respectively. There was a noted difference between theoretical and experimental values. The ratio of Ci/Cbuik for free Cd(II) by PES-N3/-imprinted functionalized silica gel were0,24.63±1.42,49.25±1.96and75.49±2.48%, respectively and were very close to the theoretical percentages of free metals in the solutions. The PES-N3/-imprinted functionalized silica gel for can accurately determine free Cd(II) in synthetic solution, while the measured value by PES-SCN/-imprinted functionalized silica gel was low. The PES-N3/-imprinted functionalized silica gel had a substantial binding capacity at pH5-8and concentrations of competitive Na+up to0.1mol·L-1. The measurements of PES-N3/-imprinted functionalized silica gel and Cd(II) ion selective electrode for free Cd(II) in river water were equivalent.
4. The PES-N3/-imprinted functionalized silica gel for can accurately determine free Cd(II) in soil. The measurements of free Cd(II) by PES-N3/-imprinted functionalized silica gel was feasible. Compared with chemical extraction method, PES-N3/-imprinted functionalized silica gel device can be used as a new tool for measurement of free Cd(II).The extraction of Imprinted functionalized silica gel for free Cd(II) is superior to other methods of morphological analysis. The results showed that the Imprinted functionalized silica gel can become a kind of new method of extracting ree Cd(II) in soil.
In summary, imprinted functionalized silica gel can used as a new tool for the quantitative measurement and sampling of free Cd(II) in soil and can provide strong technical support for assessing the environmental and health risks of heavy metals.
引文
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